Month: September 2021

In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 74534-15-9, name is 1-Chloro-2-iodo-4-nitrobenzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Safety of 1-Chloro-2-iodo-4-nitrobenzene

Procedure B was performed using N-(4-Chloro-3-iodophenyl)-6-(trifluoromethyl)-2-methylpyridine-3-carboxamide (88 mg, 0.2 mmol) with 2-pyridylzinc bromide (1 mL, 0.5 mmol, 0.5 M in THF). Purified by silica gel chromatography (10-80% ethyl acetate/hexanes) to yield N-(4-chloro-3-(pyridin-2-yl)phenyl)-6-(trifluoromethyl)-2-methylpyridine-3-carboxamide as a yellow solid: TLC Rf=0.28 (35% ethyl acetate/hexanes); TLC Rf=0.28 (35% ethyl acetate/hexanes); 1H NMR (CDCl3, 400 MHz) 8.88 (bs, 1H), 8.41 (d, 1H), 7.96 (dd, 1H), 7.74 (m, 4H), 7.52 (d, 1H), 7.22 (m, 1H), 2.75 (s, 3H); MS (Q1) 392 (M)+. An alternative synthetic procedure is as follows. 75 g (435 mmol) of 2-chloro-5-nitroaniline was added to a solution of water (600 mL) and conc. sulfuric acid (60 mL) in a 3 L 3-neck flask equipped for mechanical stirring. The solution was cooled to 0 C. and a solution of sodium nitrite (34.2 g, 496 mmol) in water (130 mL) was added slowly. The mixture was stirred for ½ hr. and then a solution of potassium iodide (130 g, 783 mmol) in water (520 mL) was added dropwise over ½ hr keeping the temperature below 15 C. The solution was stirred for 2 hr, then extracted with EtOAc (3×500 mL). The combined organic extracts were washed with sat. Na2S2O3 (2×500 mL), dried (Na2SO4), and concentrated. The crude iodide was dissolved in hot iPrOH (500 mL) and hexanes (200 mL) were added. The reaction was allowed to cool with stirring and the product was collected by suction filtration after stirring at 0 C. for 2 hr yielding 90 g (318 mmol, 73%) 2-chloro-5-nitro-iodobenzene as a light tan crystalline solid. The 2-chloro-5-nitro-iodobenzene (5 g, 17.6 mmol) was dissolved in 5 mL DMA in an oven dried flask and a 0.5M solution of 2-pyridylzincbromide (53 mL, 26.5 mmol, 0.5 M in THF) was added. The solution was degassed with N2 for ½ hr., the PPh3 (0.185 g, 0.7 mmol) and Pd(PPh3)4 (0.825 g, 0.7 mmol) were added, rinsed in with several mLs THF and the solution was degassed for a further 10 min before heating to 60 C. under N2. The reaction was complete by TLC in 8 h, cooled to RT, and poured into a 1:1 mixture of EtOAc/2.5N NaOH (500 mL). This solution was stirred for 10 min, passed through a course fritted filter containing celite to remove the solid, and then extracted. The organics were washed with brine and concentrated to a brown solid. The combined aqueous layers were backextracted with Et2O (1×200 mL). This was used to suspend the crude product, which was extracted with 1N HCl (1×200 mL, 3×100 mL). The combined aqueous extracts were cooled to 0 C., diluted with EtOAc (250 mL), and made basic with ION NaOH (100 mL). This solution was separated, the aqueous layer extracted with EtOAc, and the combined organics were dried over Na2SO4 and charcoal with stirring. This solution was filtered through celite and concentrated to yield pure 4-chloro-3-(pyridin-2-yl)nitrobenzene (2.47 g, 10.5 mmol, 60% yield) which was used in the next reaction without further purification.

The synthetic route of 74534-15-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Gunzner, Janet L.; Sutherlin, Daniel; Stanley, Mark S.; Bao, Liang; Castanedo, Georgette M.; Lalonde, Rebecca L.; Wang, Shumei; Reynolds, Mark E.; Savage, Scott J.; Malesky, Kimberly; Dina, Michael S.; US2006/63779; (2006); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 723294-75-5, In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 723294-75-5 as follows.

To a solution of 13 (50 mg, 0.2mmol) in imL of dry DMF was added 14 (53mg, 0.2mmol), C52C03 (200 mg, 0.2mmoi), Pd(dba)2 (20 mg) and Xantphos (10 mg). The mixture was degassed under vacuo and purged with N2 for several times. Then the mixture was stirred at 110C for 2h, The mixture was diluted with water (2OmL) and extracted with EtOAc (5OmL).The organic layer was washed with brine (2OmL), dried over anhydrous Na2SO4 and concentrated. The crude product was purified by prep-TLC to give the target product Compound 1 (2.8 mg, yield: 4%).LCMS: ith. 445.9(M-t-HY;1IINMR (400 MHz, CDC]3): oe857 (s, I El), .03(s, IH), ?787(s, 111), 7.82-7.83(m, IH),7 71(m IH) 7 8-7 61(m 1H) 7 54(s, 1H) 7 50-7 5(m IH) 7 47- 0 m, I H) 7 30-7 12 (m, 2H), 729-728 (m, 1H.

According to the analysis of related databases, 723294-75-5, the application of this compound in the production field has become more and more popular.

Reference:
Patent; HUA MEDICINE (SHANGHAI) LTD.; CHEN, Li; LI, Yongguo; (44 pag.)WO2017/173604; (2017); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 202982-67-0, In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 202982-67-0, name is 4-Chloro-3-fluoroiodobenzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Reference Production Example 4To a solution of 3.0 g of 2-fluoro-4-iodochlorobenzene and 3.6 g of methyl (3, 3, 3-trifluoropropylsulfonyl) acetate in 100 ml of 1,4-dioxane were added 1.40 g of sodium hydride (60% dispersion in paraffin liquid), 242 mg of (dibenzylideneacetone) (chloroform) dipalladium (0) and 368 mg of triphenylphosphine at room temperature, and the mixture was stirred at 800C for 5 days. To the reaction mixture was added 10% hydrochloric acid, followed by extraction with ethyl acetate. The organic layer was dried over anhydrous sodium sulfate and concentrated under reduced pressure. The residue was subjected to silica gel column chromatography to obtain 1.8 g of methyl (4-chloro-3- fluorophenyl) -(3,3, 3-trifluoropropylsulfonyl) acetate represented by the following formula:1H-NMR (CDCl3, TMS): delta (ppm) 7.43-7.53 (2H, m) , 7.31 (IH, dd) , 5.02 (IH, s), 3.90 (3H, s) , 3.17-3.58 (2H, m) , 2.44- 2.77 (2H, m) .

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, 4-Chloro-3-fluoroiodobenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; SUMITOMO CHEMICAL COMPANY, LIMITED; WO2009/14268; (2009); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 10297-05-9, name is 1-Chloro-4-iodobutane, belongs to iodides-buliding-blocks compound, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 10297-05-9, Recommanded Product: 10297-05-9

A)Methyl 6-chloro-2-(2-fluorophenyl)-2-(6-methoxy-3-nitropyridin-2-yl)hexanoate (XII)To 9.3 g of sodium hydride at 60percent in oil in suspension in 900 ml of DMF is added at 0° C., dropwise, the mixture of 20 g of 2-chloro-6-methoxy-3-nitropyridine and 19.6 g of methyl 2-fluorophenyl acetate in solution in 100 ml of DMF.The reaction mixture is stirred for 3 h, allowing the temperature to rise to room temperature and then 34 ml of iodochlorobutane are added.The mixture is stirred at RT for 48 h.500 ml of a 5percent aqueous NaHCO3 solution are added and the mixture is extracted with 500 ml of AcOEt.The organic phase is washed with 300 ml of a 5percent aqueous NaHCO3 solution, dried over Na2SO4 and then the solvents are then evaporated under reduced pressure.The residue is purified by silica gel chromatography, eluting with a cyclohexane/ethyl acetate mixture to give the expected compound in the form of a liquid which is used as it is in the next step.

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it.

Reference:
Patent; SANOFI-AVENTIS; US2011/71160; (2011); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 5458-84-4, name is 1-Iodo-2-methoxy-4-nitrobenzene, A new synthetic method of this compound is introduced below., Product Details of 5458-84-4

Method 2 A solution of 1-iodo-2-methoxy-4-nitrobenzene (15 g, 53.8 mmol), DIPEA (30 ml_, 172 mmol) and ethyl methylphosphinate (9.51 ml_, 64.8 mmol) in toluene (100 ml_) was vacuum degassed and back filled with N2 three times. The reaction mixture was warmed to 50C. XantPhos G3 precatalyst (1 g, 1.056 mmol) was added and the reaction heated under N2 at 85C (internal temperature, 100C block temperature) for 1 h. The reaction mixture was cooled, preabsorbed onto silica (9.9 g) and purified by chromatography on silica gel (40 g column, 50% EtOAc: isohexane to 100%) to afford the sub-title compound (10 g) as a pale tan solid. 1 H NMR (400 MHz, DMSO-d6) delta 8.02 (dd, 1 H), 7.94 (dt, 1 H), 7.88 (dd, 1 H), 4.01 (s, 3H), 3.98 – 3.85 (m, 1 H), 3.81 – 3.68 (m, 1 H), 1.71 (d, 3H), 1.16 (t, 3H). LCMS m/z 260 (M+H)+ (ES+)

The synthetic route of 5458-84-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; RESPIVERT LIMITED; TOPIVERT PHARMA LIMITED; BAKER, Thomas Matthew; FYFE, Matthew Colin Thor; JONES, Geraint; THOM, Stephen Malcolm; (270 pag.)WO2016/51187; (2016); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Some common heterocyclic compound, 249647-24-3, name is Methyl 3-bromo-4-iodobenzoate, molecular formula is C8H6BrIO2, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route. Recommanded Product: Methyl 3-bromo-4-iodobenzoate

Example 31Preparation of lambda/-r2-amino-1-(phenylmethyl)ethyll-3-bromo-4-(1-methyl-1/-/-pyrazol- 5-yl)benzamidea) methyl 3-bromo-4-(1-methyl-1 /-/-pyrazol-5-yl)benzoateTo a solution of methyl 3-bromo-4-iodobenzoate (409 mg, 1.2 mmol) in dioxane/H2O (4:1 , 10 ml.) was added K2CO3 (497 mg, 3.6 mmol), tetrakistriphenylphosphine Pd(O) (69 mg, 0.06 mmol) and 5-(5,5-dimethyl-1 ,3,2- dioxaborinan-2-yl)-1-methyl-1 /-/-pyrazole (349 mg, 3.6 mmol). The reaction mixture was heated to 80 C in a sealed tube for 12h and was then partitioned between 6N NaOH and DCM. The pH of the aqueous phase was adjusted to ~3 with 3M HCI and washed several times with DCM. The combined organic fractions were dried (Na2SO4), concentrated under vacuum and used directly without further purification (307 mg, 87%): LC-MS (ES) m/z = 296 (M+H)+.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 249647-24-3, its application will become more common.

Reference:
Patent; SMITHKLINE BEECHAM CORPORATION; WO2008/121786; (2008); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 626-44-8 as follows. Recommanded Product: 1,3,5-Triiodobenzene

Synthesis of 1 , 3 , 5-tris [( 1 , 3-diethylcarboxylate-5- ( 4- (ethynyl ) phenyl )) butadiynyl ] -benzene (compound 6). 1,3,5- Triiodobenzene (5, 1.1 g, 2.41 mmol), compound 4 (3.0 g, 11.1 mmol), THF (100 ml), and diisopropylamine (50 ml) are combined in a 500 mL Schlenk flask equipped with a magnetic stir bar and a rubber stopper. The mixture is cooled to -78 °C in an acetone/dry ice bath and subjected to three cycles of brief vacuum-degas/N2 back-fill with no stirring. Then Pd(PPh3)4 (450 mg, 0.39 mmol) and Cul (150 mg, 0.79 mmol) is added to this degassed solution under positive N2 flow and the mixture is degassed for three more cycles. The solution is stirred for 48 h at 25 °C, concentrated, and dried under high vacuum. The remaining brown paste is redissolved in a minimum amount of CHCI3, and column chromatographed over silica gel using CHCI3 (stabilized with 2percent ethanol) to give a brown solid (2.1 g) , which is recrystallized three times from CHCl3:EtOH (75 ml, 2:1, v/v) to give the product 6 as an off-white solid. Yield = 1.7 g (80percent). XH NMR (500 MHz, CDC13) is shown in Fig. 16, where delta 1.42 (t, J = 7.0 Hz, 18H, -C02CH2C) , 4.43 (q, J = 7.0 Hz, 12H, -C02Cfi2CH3) , 7.65 (s, 3H, Ar2-fi) , 8.35 (d, J = 1.5 Hz, 6H, Ari-H) , 8.67 (t, J = 1.5 Hz, 3H, Ari-H) . 13C NMR (126 MHz, CDCI3) is shown in Fig. 17, where delta 14.43, 61.88, 75.13, 75.50, 79.78, 80.63, 122.45, 123.00, 131.29, 131.60, 136.72, 137.36, and 164.92.

According to the analysis of related databases, 626-44-8, the application of this compound in the production field has become more and more popular.

Reference:
Patent; NORTHWESTERN UNIVERSITY; FARHA, Omar, K.; HUPP, Joseph, T.; WILMER, Christopher, E.; ERYAZICI, Ibrahim; SNURR, Randal, Q.; GOMEZ-GUALDRON, Diego, A.; BORAH, Bhaskarjyoti; WO2013/192146; (2013); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 391211-97-5, name is 3,4-Difluoro-2-((2-fluoro-4-iodophenyl)amino)benzoic acid belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Application In Synthesis of 3,4-Difluoro-2-((2-fluoro-4-iodophenyl)amino)benzoic acid

A solution of 3,4-difluoro-2-[(2-fluoro-4-iodophenyl)amino]benzoic acid (200 mg, 0.51 mmol), prepared using procedures similar to those in US 7,019,033, PyBOP (256 mg, 0.51 mmol), commercially available tert-butyl azetidin-3-ylcarbamate (131 mg, 0.77 mmol) and lambdazetaiV-diisopropylethylamine (180 muL, 1.02 mmol) in dimethylformamide (3 mL) was stirred at room temperature for 15 hours. The reaction mixture was partitioned between 5% aqueous lithium chloride and ethyl acetate. The organic portion was washed with 20% aqueous citric acid, saturated aqueous sodium bicarbonate, brine, dried over sodium sulfate, filtered and concentrated in vacuo to afford a brown residue which was purified by silica gel column chromatography eluting with 30% ethyl acetate in hexanes to afford 1,1- dimethylethyl [ 1 -( { 3 ,4-difluoro-2- [(2-fluoro-4-iodophenyl)amino]phenyl } carbonyl)azetidin- 3-yl]carbamate (225 mg, 80% yield) as a colorless oil. 1H NMR (400 MHz, DMSO): 8.56 (s, IH), 7.60-7.55 (m, 2H), 7.38 (d, IH), 7.30-7.26 (m, IH), 7.20-7.13 (m, IH), 6.71-6.66 (m, IH), 4.37-4.20 (m, 2H), 4.18-4.06 (m, IH), 3.98-3.93 (m, IH), 3.82-3.75 (m, IH), 1.37 (s, 9H). MS (EI) C2IH21N3O3F3I: 548 (MH+).

The synthetic route of 391211-97-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; EXELIXIS, INC.; WO2008/124085; (2008); A2;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 2043-57-4, name is 1,1,1,2,2,3,3,4,4,5,5,6,6-Tridecafluoro-8-iodooctane, A new synthetic method of this compound is introduced below., Safety of 1,1,1,2,2,3,3,4,4,5,5,6,6-Tridecafluoro-8-iodooctane

2.4. Synthesis of 1-chloro-3-1H,1H,2H,2H-perurooctyl-5,5-dimetylhydantoin (Cl-FODMH)3-1H,1H,2H,2H-perurooctyl-5,5-dimetylhydantoin (FODMH)was synthesized using similar procedures as in the preparation ofODMH. Briey, 3.20 g DMH were dissolved in 30 mL methanol inthe presence of 1.68 g potassium hydroxide. The mixture was keptat 50 C for 30 min. After evaporation of the solvent, the potassiumsalt of DMH was dried in a vacuum oven at 60 C for three days. Theanhydrous salt was then dispersed in 100 mL N,N-dime-thylformamide (DMF) at 95 C for 10 min under constant stirring,after which 11.85 g IFO were added into the mixtures. The reactionwas continued for 4 h at 95 C. At the end of the reaction, theformed KI was ltered off. After the removal of DMF by distillationunder reduced pressure, the residual substance was recrystallizedfrom ethanol. 3-1H,1H,2H,2H-perurooctyl-5,5-dimetylhydantoin(FODMH) was obtained as white powders with a yield of 60.7%(7.22 g).In the preparation of Cl-FODMH, 0.5 g FODMH and 0.74 g tri-chloroisocyanuric acid (TCCA) were dissolved in acetone [10]. Here,TCCA was employed because our screening tests showed that usingchlorine bleach as the chlorination agent could not chlorinateFODMH successfully due to the very hydrophobic nature ofFODMH. The solution was vigorously stirred for 30 min at ambienttemperature. At the end of the reaction, acetone was evaporated,hexane was added to the mixtures, and the insoluble solids wereltered off. After removing hexane from the ltrate by evaporation,Cl-FODMH was obtained as white powders with a yield of 59.2%.

The synthetic route of 2043-57-4 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Lin, Jiajin; Jiang, Fuguang; Wen, Jianchuan; Lv, Wei; Porteous, Nuala; Deng, Ying; Sun, Yuyu; Polymer; vol. 68; (2015); p. 92 – 100;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 391211-97-5, name is 3,4-Difluoro-2-((2-fluoro-4-iodophenyl)amino)benzoic acid, A new synthetic method of this compound is introduced below., Computed Properties of C13H7F3INO2

1 , 1 -Dimethylethyl 3 -hydroxy-3 -(2-methyl- 1 -nitropropyl)azetidine- 1 -carboxylate (105 mg, 0.38 mmol) was taken into methanol (1 mL) followed by addition of 4 N anhydrous hydrogen chloride in dioxane (1 mL) and the acidic solution was allowed to stand for 15 minutes at room temperature then concentrated and dried in vacuo to an amorphous residue. 3,4-Difluoro-2-[(2-fluoro-4-iodophenyl)amino]benzoic acid (150 mg, 0.38 mmol), prepared using procedures similar to those described in US 7,019,033, was taken into DMF (0.7 mL) followed by addition of PyBOP (198 mg, 0.38 mmol) and the solution was allowed to stir for 10 minutes at room temperature. The above amine hydrochloride salt and DIPEA (190 muL, 1.1 mmol) in DMF solution (0.7 mL) was added and the mixture was allowed to stir for one hour at room temperature. The mixture was partitioned with ethyl acetate and 0.5 N aqueous EPO hydrochloric acid and the organic phase washed three times with water then brine and dried over anhydrous magnesium sulfate. Filtration and concentration afforded a residue that was further purified by silica gel flash chromatography using 1.5:1 hexanes:ethyl acetate as eluent to give l-({3,4-difluoro-2-[(2-fluoro-4-iodophenyl)amino]phenyl}carbonyl)-3-(2-methyl-l- nitrorhoropyl)azetidin-3-ol (189 mg, 90% yield) as an amorphous solid. 1H-NMR (400 MHz, CDCl3): 8.41 (br s, IH), 7.41 (dd, IH), 7.34 (d, IH), 7.09 (br m, IH), 6.81 (q, IH), 6.65-6.60 (m, IH), 4.49 (d, IH), 4.15-4.09 (m, 4H), 3.66 (s, IH), 2.56-2.46 (m, IH) 1.03 (d, 6H).

The synthetic route of 391211-97-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; EXELIXIS, INC.; WO2007/44515; (2007); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com