Month: October 2020

112671-42-8, 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. 112671-42-8, name is 4-Bromo-1-iodo-2-nitrobenzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

In the round bottom flask, the benzo [b] thiophene-3- base boric acid (benzo[b]thiophen-3-ylboronicacid) 65.1g, 4-bromo-1-iodo-2-nitrobenzene (4-bromo-1-iodo-2-nitrobenzene) 100g dissolving in toluene 1600 ml and adding K2CO3(2M) 455 ml and Pd (PPh3)4(four (triphenylphosphine) palladium) 10.5g of the backflow after stirring. In TLC (thinlayerchromatography, thin layer chromatography) confirmed the reaction and the reaction is terminated after addition of water. The organic layer using EA and extraction (ethanol) of the pressure-reducing filter after the column to purify 84.5g intermediate 4′ -1 (the yield is 83%).

The synthetic route of 112671-42-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Xian, hao wan; an, xianzhe; han, zheng you; jin, jin tai; li, ying zhen; (67 pag.)CN105473594; (2016); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

612-55-5, Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 612-55-5, name is 2-Iodonaphthalene, This compound has unique chemical properties. The synthetic route is as follows.

General procedure: Aryl iodide 3 (0.2 mmol, 1.0 equiv), acrylate/styrene 4 (0.202 mmol, 1.01 equiv), DIPEA (28.4 mg, 0.22 mmol, 1.1 equiv), and Pd(I)-iodo dimer 2 (1.3 mg, 0.0015 mmol, 0.75 mol%) were weighed into a 4 mL screw cap vial, purged with argon, and dissolved in anhydrous toluene(1.5 mL). The vial was capped with a PTFE-lined screw cap and sealed with PTFE tape prior to heating to 100 C under stirring by using an aluminum heating block outside the glovebox. After 15 h, the reaction mixture was allowed to cool to r.t. and diluted with EtOAc (to 20 mL); excess base was quenched by the addition of sat. aq NH4Cl (20 mL). The organic phase was separated and the aqueous layer was extracted with EtOAc (2*20 mL). The combined organic layer was dried over MgSO4 and the solvent was removed under reduced pressure. The obtained crude product was purified by flash column chromatography.

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:
Article; Sperger, Theresa; Stirner, Christopher K.; Schoenebeck, Franziska; Synthesis; vol. 49; 1; (2017); p. 115 – 120;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

116632-39-4, Adding a certain compound to certain chemical reactions, such as: 116632-39-4, name is 5-Bromo-2-iodotoluene, 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 116632-39-4.

General procedure: To a stirred solution of 6-bromo-3-pyridyl boronic acid (1.25 equiv, 847 mg, 4.20 mmol) in 1,4-dioxane (30 mL) under nitrogen were added 5-bromo-2-iodotoluene (1 g, 3.36 mmol) and tetrakis-(triphenylphosphine)palladium(0) (0.05 equiv, 195 mg, 0.17 mmol). After 5 min of stirring, aqueous Na2CO3 (2.5 equiv, 892 mg, 8.42 mmol) in 5 mL of water was added. Then the mixture was heated to 80 C until the starting material was consumed (TLC). After cooling down to room temperature, the mixture was filtered on Celite and washed with CH2Cl2. The aqueous layer was extracted with EtOAc (2¡Á50 mL). Combined organic layers were washed with saturated aqueous solution of NaCl (50 mL), and dried over MgSO4. Solvent was removed in vacuo and crude product was purified by column chromatography, with 99:1 cyclohexane/EtOAc affording 3c as a white solid (520 mg, 47%).

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, 5-Bromo-2-iodotoluene, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Perato, Serge; Voisin-Chiret, Anne Sophie; Sopkova-De Oliveira Santos, Jana; Legay, Remi; Oulyadi, Hassan; Rault, Sylvain; Tetrahedron; vol. 68; 7; (2012); p. 1910 – 1917;,
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 1878-69-9 as follows. 1878-69-9

2- (3-LODOPHENYL) ETHANOL; A solution of borane (1 M, THF, 2.5 eq. , 38.2 mL) was added dropwise to a stirred solution of (3-iodophenyl) acetic acid (4.0 g) in THF (100 mL) cooled to 0 OC. The resulting mixture was stirred at 0 oC for 1H then warmed to room temperature and stirred for a further 3 h. The mixture was poured into aqueous ammonium chloride solution and extracted with ethyl acetate. The combined organic phases were washed with brine, dried (sodium sulfate) and concentrated. The crude was purified by column chromatography (SPE cartridge, SIO2), using cyclohexane-ethyl acetate (70: 30) as eluent to afford the title compound (3.5 g, 92 % yield). 1H-NMR (400 MHz, CDC . S) 5 (ppm): 7.5-7 (m 5H), 4.0 (m, 2H), 2.9 (m, 2H).

According to the analysis of related databases, 1878-69-9, the application of this compound in the production field has become more and more popular.

Reference:
Patent; GLAXO GROUP LIMITED; WO2005/14552; (2005); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

364-77-2, A common compound: 364-77-2, name is 2-Iodo-5-fluoronitrobenzene, belongs to iodides-buliding-blocks compound, it can change the direction of chemical reaction, and react with certain compounds to generate new functional products. A new synthetic method of this compound is introduced below.

A solution of 4-fluoro-1-iodo-2-nitrobenzene 1 (Oakwood Products, 2.403 g, 9.00 mmol), triphenylphosphine (1.416 g, 5.40 mmol), dry Et3N (1.88 mL, 13.5 mmol), Pd(OAc)2 (303.1 mg, 1.35 mmol), and methyl acrylate (1.62 mL, 18.0 mmol) in dry DMF (24.0 mL) was stirred at 130 C under N2 for 9 h. The reaction solution was cooled to room temperature, and concentrated in vacuo. The residue was partitioned between AcOEt/toluene solution (1:2, 60 mL) and H2O (50 mL). The organic layer was separated and the aqueous layer was extracted with AcOEt/toluene solution (1:3, 40 mL ¡Á 3). The organic layers were combined, dried over anhydrous MgSO4, filtered, and concentrated in vacuo. The residue was purified by flash column chromatography (silica gel, hexane/AcOEt = 5:1) to afford 286.7 mg of the title product 3 in 14% yield as a yellow crystalline solid. 1H NMR (270 MHz, CDCl3) delta 8.07 (1H, d, 15.8 Hz), 7.78 (1H, dd, J = 8.07 Hz, J = 2.65 Hz), 7.68-7.63 (1H, m), 7.43-7.38 (1H, m), 6.34 (1H, d, J = 15.8 Hz), 3.84 (3H, s).

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, 2-Iodo-5-fluoronitrobenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Hayashi, Shigeo; Ueno, Naomi; Murase, Akio; Nakagawa, Yoko; Takada, Junji; European Journal of Medicinal Chemistry; vol. 50; (2012); p. 179 – 195;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

A common heterocyclic compound, 39998-81-7, name is 2-Fluoro-4-iodo-1-methylbenzene, molecular formula is C7H6FI, its 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. 39998-81-7.

2-Fluoro-4-iodotoluene (2.83 g, 12 mmol) was added to a 250 mL round bottom flask and dissolved in carbon tetrachloride (120 mL).NBS (2.24 g, 12.6 mmol) and BPO (0.06 g, 0.24 mmol) were added to the solution under stirring, and the reaction system was heated to reflux for 9 h under nitrogen protection.After the reaction is completed, it is cooled to room temperature, and the reaction solution is evaporated under reduced pressure to remove the solvent.The crude product was purified by column chromatography (eluting with petroleum ether) to give a white solid (2.16 g, 57%).

The synthetic route of 2-Fluoro-4-iodo-1-methylbenzene has been constantly updated, and we look forward to future research findings.

Reference:
Patent; SUNSHINE LAKE PHARMA CO., LTD.; ZHANG, YINGJUN; ZHANG, JIANCUN; WANG, XIAOJUN; LIN, RUNFENG; CAO, SHENGTIAN; WANG, ZHAOHE; LI, JING; (226 pag.)TWI607995; (2017); B;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

82998-57-0, name is 3-Iodo-4-methylbenzoic acid, belongs to iodides-buliding-blocks compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. 82998-57-0

3-Iodo-4-methylbenzoic acid (lOg, 38.16mmol), bis (pinnacolato) diboron (14.5g, 57. 24mmol), potassium acetate (18.73g, 190.8mmol) and PdCl2dppf (3.12g, 3.8mmol) in DMF (200ml) were heated at 80C for 21hrs. The solvent was evaporated from the cooled reaction under vacuum, the residue dissolved in ethyl acetate (300ml) and hydrochloric acid (2N, 300ml) and filtered through celite. The organic phase was separated and the aqueous extracted with ethyl acetate (2 x 300ml). The combined organic extracts were washed with brine (500ml) and dried (magnesium sulphate). The solvent was evaporated under vacuum and the residue was absorbed onto silica and applied to a silica column. This was eluted with cyclohexane/ethyl acetate (5: 1). to give the title compound. NMR: AH [d6-DMSO] 12.83, (1H, b), 8.23, (1H, d), 7.89, (1H, dd), 7.29, (1H, d), 2.51, (3H, s), 1.30, (12H, s). LCMS: Rt 3. 65min.

Statistics shows that 82998-57-0 is playing an increasingly important role. we look forward to future research findings about 3-Iodo-4-methylbenzoic acid.

Reference:
Patent; SMITHKLINE BEECHAM CORPORATION; WO2004/10995; (2004); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 672-57-1 name is 1-Chloro-2-iodo-4-(trifluoromethyl)benzene, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below. 672-57-1

General procedure: The corresponding iodobenzenederivative 14a or 14b (1.80 mmol) and 5-formyl furan-2-ylboronicacid 15 (2.34 mmol) were dissolvedin 10 mL DMF and 15 mL EtOH. The reaction mixture was stirred for 10 min underN2, then Pd(PPh3)2Cl2 (0.18 mmol)and a solution of Na2CO3 (2M, 10.8 mmol) were added to thereaction mixture, and the light-orange suspension was stirred under N2at room temperature. After 1 h the reaction went to completion (TLC) and wasquenched with 1M HCl, then EtOAc (10 mL) was added, and the mixture was stirreduntil the two layers became clear. The combined organic layers were washed withH2O and brine, dried over Na2SO4, filtered,and evaporated under reduced pressure. The crude product was purified by flashchromatography using PE/EtOAc as eluent to yield the desired product as a solid(yields: 8 (64%), 13 (87%)).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1-Chloro-2-iodo-4-(trifluoromethyl)benzene, and friends who are interested can also refer to it.

Reference:
Article; Botta, Lorenzo; Maccari, Giorgio; Calandro, Pierpaolo; Tiberi, Marika; Brai, Annalaura; Zamperini, Claudio; Canducci, Filippo; Chiariello, Mario; Marti-Centelles, Rosa; Falomir, Eva; Carda, Miguel; Bioorganic and Medicinal Chemistry Letters; vol. 27; 11; (2017); p. 2502 – 2505;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

2401-21-0, Name is 1,2-Dichloro-3-iodobenzene, 2401-21-0, belongs to iodides-buliding-blocks compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows.

EXAMPLE 4 200 mg of 3-alpha-cholestanyl nicotinate (0.4 mmoles) and 130 mg of iodobenzenedichloride were dissolved in 19 ml of dichloromethane. 200 ml of epoxybutane (2.3 mmoles) was added as a hydrogen chloride scavenger and the solution was irradiated with a sunlamp for 10 minutes. 9-chloro-3-alpha cholestanyl nicotinate was isolated by evaporating the solvent and was purified on a silica column.

Statistics shows that 1,2-Dichloro-3-iodobenzene is playing an increasingly important role. we look forward to future research findings about 2401-21-0.

Reference:
Patent; The Trustees of Columbia in the City of New York; US4920216; (1990); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

A common compound: 2043-55-2, name is 1,1,1,2,2,3,3,4,4-Nonafluoro-6-iodohexane, belongs to iodides-buliding-blocks compound, it can change the direction of chemical reaction, and react with certain compounds to generate new functional products. A new synthetic method of this compound is introduced below. 2043-55-2

Preparation of [CF3 (CF213CH2CH2LO-3H2] A mixture of 37.4 g of [1-IODO-LH, LH,] 2H, [2H-PERFLUOROHEXANE] and 50.0 g of triethyl phosphite was heated at [150 ¡ãC.] After 16 hr, an additional 50.0 g of triethyl phosphite was added, and heating was continued. After 2 hr, an additional 50.0 g of triethyl phosphite was again added, and heating was continued for another 24 hr. Diethyl ethylphosphonate and other volatiles were removed by distillation through a 12-inch (30 cm) vacuum- jacketed packed column, b. p. [34-38 ¡ãC] at 0.05 torr (7 Pa). Distillation of the concentrate provided 22.3 g of [1-DIETHYLPHOSPHONO-LH, LH,] 2H, 2H-perfluorohexane as a 90: 2: 7 mixture with triethyl phosphate and ethyl 1H, lH, 2H, 2H-perfluorohexyl ethylphosphonate as a clear, colorless liquid, b. p. [47-51 ¡ãC] at 0.05 torr (7 Pa).

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, 2043-55-2, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; 3M INNOVATIVE PROPERTIES COMPANY; WO2003/102003; (2003); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com