Month: February 2021

Related Products of 52548-63-7, A common heterocyclic compound, 52548-63-7, name is 5-Fluoro-2-iodobenzoic acid, molecular formula is C7H4FIO2, 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.

General procedure: A mixture of the appropriate benzoic acid (10.0 mmol) and oxalyl chloride (15 mmol) was stirred at 0C for 2 h. The oxalyl chloride was removed under reduced pressure.

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Reference:
Article; Kong, Lu-Lu; Fan, Li-Yan; Chinese Chemical Letters; vol. 27; 6; (2016); p. 827 – 831;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 626-62-0, name is Iodocyclohexane, 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 626-62-0, Application In Synthesis of Iodocyclohexane

In a round bottomed 500 ml flask equipped with stir bar and containing 100 ml acetone, was added 7.6 g of ammonium thiocyanate salt and stirred at room temperature until the complete dissolution of salt. To this clear solution, 10 g of montmorillonite K10 clay was added in portions over 10 min with stirring. After complete addition, the formation of reddish suspension was observed which was vigorously stirred for another 30 min at room temperature. Then the suspension is placed in a rotary vacuum evaporator and the solvent was removed under reduced pressure. The dry solid crust adhering to the walls of the flask was flaked off with a spatula, and solvent evaporation was resumed. After complete drying, yielded, about 17.6 g of clay supported ammonium thiocyanate as a light red free flowing powder which shows no loss of reactivity after standing in an open powder box for one week.; Phenacyl bromide (1 mmol) and K10-montmorillonite clay supported ammonium thiocyanate (3 mmol) were taken in mortar, mixed with spatula, and ground with pestle for stipulated time (see Table 3). After complete conversion as indicated by TLC, the solid reaction mixture was directly loaded on silica gel column by avoiding aqueous work up-extraction step. Later elution with ethyl acetate-hexane (9:1-3:1) solvent system and evaporation of solvents in rotary vacuum evaporator afforded pure phenacyl thiocyanate (99%). Same procedure as discussed above was followed to prepare all thiocyanate compounds shown in this work. All compounds prepared were characterized by IR, Mass, and NMR spectroscopy.

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, Iodocyclohexane, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Meshram; Thakur, Pramod B.; Madhu Babu; Bangade, Vikas M.; Tetrahedron Letters; vol. 53; 14; (2012); p. 1780 – 1785;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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. 69113-59-3, name is 3-Iodobenzonitrile, This compound has unique chemical properties. The synthetic route is as follows., Safety of 3-Iodobenzonitrile

General procedure: General procedure: An oven-dried Schlenk tube containing a magnetic stirring bar was charged with methyl 4-iodobenzoate 2a (52.40 mg, 0.2 mmol), Pd(OAc)2 (2.24 mg, 0.01 mmol) and Ag2CO3 (55.15 mg, 0.2 mmol) under nitrogen. To this mixture was added trimethyl(2-phenylallyl)silane 1a (57.11 mg, 0.3 mmol) and DCE (4 ml) by a syringe. After the reaction completed, it was quenched by saturated NaHCO3 aqueous solution. The mixture was extracted by DCM. Then the combined organic extracts were washed with brine, dried over Na 2 SO 4 and filtered. After concentration, the residue was submitted to flash chromatography on a silica gel column with petroleum ether/dichloromethane (5:1) as the eluent to give the product 3aa as a white solid.

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of 69113-59-3.

Reference:
Article; Hou, Zhen-Lin; Yang, Fan; Zhou, Zhibing; Ao, Yu-Fei; Yao, Bo; Tetrahedron Letters; vol. 59; 52; (2018); p. 4557 – 4561;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 82998-57-0,Some common heterocyclic compound, 82998-57-0, name is 3-Iodo-4-methylbenzoic acid, molecular formula is C8H7IO2, 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.

REFERENCE EXAMPLE 19; 4-Methyl-3-(4,4,5,5-tetramethyl[1 ,3,2]dioxaborolan-2-yl)benzoic acid; To a solution of 3-iodo-4-methylbenzoic acid (3.71 g, 14.2 mmol) in DMF (130 mL), bis(pinacolato)diboron (7.20 g, 28.4 mmol), [1 ,1′-bis(diphenylphosphino) EPO ferrocene]dichloro-palladium (II) (1.04 g, 1.28 mmol) and potassium acetate (6.95 g, 70.9 mmol) were added under argon. The mixture was heated at 80 0C overnight and then allowed to cool to room temperature. The solvent was evaporated and the residue was diluted with water and EtOAc. The phases were separated and the aqueous phase was extracted with EtOAc. The combined organic phases were washed twice with 3N HCI and dried over Na2SO4. The solvent was evaporated and the crude product thus obtained was purified by chromatography on silica gel using hexane-EtOAc mixtures of increasing polarity as eluent, to afford the title compound impurified with starting bis(pinacolato)diboron. The product was slurried in hexane, filtered and dried under vacuum to afford 2.41 g of pure material (yield: 65%). 1H NMR (300 MHz1 CDCI3) delta (TMS): 1.36 (s, 12 H), 2.61 (s, 3 H)1 7.25 (d, J = 8.1 Hz1 1 H), 8.02 (dd, J = 8.1 Hz1 J1 = 2.1 Hz, 1 H)1 8.48 (d, J = 2.1 Hz, 1 H). LC-MS (method 1): tR = 7.57 min; m/z = 261.0 [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 3-Iodo-4-methylbenzoic acid, its application will become more common.

Reference:
Patent; J. URIACH Y COMPANIA S.A.; WO2007/339; (2007); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 1643-29-4, name is 3-(4-Iodophenyl)propanoic acid, 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 1643-29-4, Recommanded Product: 3-(4-Iodophenyl)propanoic acid

A suspension of 3-(4-iodophenyl)propanoic acid (19) (0.50 g,1.81 mmol), bis(pinacolato)diboron (0.69 g, 2.72 mmol), and KOAc(0.71 g, 7.24 mmol) in DMF (1 ml) was degassed by bubbling argon through the mixture for 15 min, then Pd(dppf)Cl2 (66 mg,0.09 mmol) was added to this mixture. The reaction was heated to 80 C for 2.5 h. The reaction mixture was cooled to rt, filtered through a pad of silica gel, and washed with EtOAc. The filtrate was concentrated under reduced pressure and purified by column chromatography on silica gel (EtOAc in petroleum ether, 1:2) to give the product 20 (0.32 g, 63%) as a white solid. 1H NMR(300 MHz, CDCl3) d: 10.43 (b s, 1H), 7.75 (d, J = 8.0 Hz, 2H), 7.22(d, J = 8.0 Hz, 2H), 2.98 (t, J = 7.8 Hz, 2H), 2.68 (t, J = 7.8 Hz, 2H),1.34 (s, 12H). LCMS (ESI) m/z: 277.09 [M+H]+.

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; Bobileva, Olga; Ikaunieks, Martins; Duburs, Gunars; Mandrika, Ilona; Petrovska, Ramona; Klovins, Janis; Loza, Einars; Bioorganic and Medicinal Chemistry; vol. 25; 16; (2017); p. 4314 – 4329;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 696-41-3,Some common heterocyclic compound, 696-41-3, name is 3-Iodobenzaldehyde, molecular formula is C7H5IO, 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.

Example 1A ethyl (2E)-3-(3-iodophenyl)acrylate To a suspension of NaH (60% dispersion in mineral oil) (120 mg, 3.0 mmol) in THF (20 mL) was added triethyl phosphonoacetate (436 muL, 2.2 mmol) dropwise. 3-iodo-benzaldehyde (465 mg, 2.0 mmol) was added after the bubbling has stopped. The reaction mixture was stirred at room temperature for 15 minutes. Solid NH4Cl was added, followed by 1N HCl to quench the reaction. The mixture was taken up in ethyl acetate and water. The organic phase was washed with aqueous NaHCO3, brine, dried (MgSO4), filtered and concentrated under reduced pressure and purified by flash chromatography on silica gel with hexane/ethyl acetate (4:1) to provide the titled compound (605 mg).

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

Reference:
Patent; Xin, Zhili; Liu, Gang; Pei, Zhonghua; Szczepankiewicz, Bruce G.; Serby, Michael D.; Zhao, Hongyu; US2004/167188; (2004); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 6940-76-7, 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. 6940-76-7, name is 1-Chloro-3-iodopropane belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

10.16g(50mmol) of 2-(3′,4′ -dimethoxyphenyl)-3-methylbutyronitrile was dissolved in 80ml of anhydrous toluene, and 3.90g(100mmol) of sodium amide was added in fractional amounts while being stirred. After being heated and refluxed at 120 C for 2 hours, the mixture was cooled down to 80C and, with 15.33g(75mmol) of 1-chloro-3-iodopropane added thereto, further stirred at 80 C for 1 hour. After disappearance of the starting material was checked, a small amount of methanol was added to the mixture to decompose excess sodium amide, and the solvent was evaporated out under a vacuum. The residue was extracted with ethyl acetate and then washed with water until it became neutral. The organic layer was filtrated through 1PS filter paper, and then the solvent was evaporated out. The residue was purified by silica gel column chromatography, to give 12.03g(41mmol, 81%) of 5-chloro-2-(3′,4′ -dimethoxyphenyl)-2-isopropylpentanenitrile. 1H-NMR (d, CDCl3):0.82 (3H, d, J=6.7Hz), 1.21 (3H, d, J=6.7Hz), 1.38-1.54 (1H, m), 1.80-1.98 (1H, m), 2.00-2.30 (3H, m), 3.45-3.54 (2H, m), 3.89 (3H, s), 3.90 (3H, s), 6.82-6.96 (3H, m).

The synthetic route of 1-Chloro-3-iodopropane has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Shiseido Co., Ltd.; EP1488776; (2004); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 69113-59-3, name is 3-Iodobenzonitrile, 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 69113-59-3, Recommanded Product: 3-Iodobenzonitrile

One equivalent of a substituted aromatic or heteroaromatic nitrile (here a compound of formula II, wherein R1 is phenyl, R7 is I1 X is (CH2)P and p = 0) is dissolved in 1 ,4-dioxane. After addition of 1 ,3 equivalents of a straight or branched chain alcohol of formula III (wherein R9 is (CH2)q and q is 1 – 10), HCI-gas is introduced at 1O0C for 6h. The resulting pellet (compound of formula IV) is filtered, washed with dioxane and dried in vacuum. EPO IVa) 3-lodo-benzimidic acid ethyl ester hydrochloride: 6.05 g (81%), colourless powder; HPLC: 2.11 min; LC-MS: 262.0 m/z.

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, 3-Iodobenzonitrile, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; MERCK PATENT GMBH; WO2006/131186; (2006); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 2468-56-6, 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. 2468-56-6, name is 6-Iodohex-1-yne belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

To a stirred solution of N-(2-methyl-5′-(piperazin-l-yl)-6′-((tetrahydro-2H-pyran-4- yl)oxy)-[3,3′-bipyridin]-5-yl)-3-(trifluoromethyl)benzamide (22 mg, 0.041 mmol) in DMF (0.5 mL) was added potassium carbonate (8.4 mg, 0.061 mmol) and the mixture was stirred at rt for 10 min. Then, 6-Iodo-l-hexyne (7.5 uL, 0.057 mmol) was added. The mixture was stirred at rt for 65 h, diluted with water and saturated aqueous solution of ammonium chloride. After being stirred for 5 min, the mixture was diluted with EtOAc. The phases were separated and the aqueous layer was extracted twice with EtOAc. The combined organics were washed with brine, dried over sodium sulfate, and concentrated. The residue was purified by flash chromatography on silica gel using a gradient of methanol in DCM (0-15%) to afford the title compound (16 mg, 63%) as a white solid. MR (600 MHz, CDCb) delta 8.63 (d, J = 2.0 Hz, 1H), 8.35 (s, 1H), 8.16 (s, 1H), 8.12 – 8.07 (m, 2H), 7.82 (d, J = 7.7 Hz, 1H), 7.71 (d, J = 1.4 Hz, 1H), 7.64 (t, J = 7.8 Hz, 1H), 7.03 (d, J = 1.3 Hz, 1H), 5.44 – 5.36 (m, 1H), 4.03 – 3.92 (m, 2H), 3.75 – 3.63 (m, 2H), 3.19 (s, 4H), 2.66 (s, 4H), 2.49 (s, 3H), 2.47 – 2.41 (m, 2H), 2.27 – 2.21 (m, 2H), 2.18 – 2.11 (m, 2H), 1.93 – 1.83 (m, 3H), 1.72 – 1.63 (m, 2H), 1.61 – 1.54 (m, 2H). LRMS (m/z) calculated, 621.292; found, 624.8 (M+H)+.

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, 6-Iodohex-1-yne, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; QUARTZ THERAPEUTICS, INC.; ZAMBONI, Robert; HENNING, Ryan; JI, Alan; SMITH, Tyler; HELLER, Bradley; REDDY, Thumkunta Jagadeeswar; ROCHELEAU, Sylvain; BEAULIEU, Marc Andre; (266 pag.)WO2018/200981; (2018); 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. 144-48-9, name is 2-Iodoacetamide, A new synthetic method of this compound is introduced below., Recommanded Product: 144-48-9

To a solution of 4-aminomethyl-3-hydxoxy-benzonitrile hydrochloride (BB1, 2.0 g) and triethylamine (2.19 g) in dichloromethane (20 ml) was added di-tert-butyldicarbonate (2.41 g). The mixture was stirred at r.t. for 3.5 h. The mixture was washed with water (3x), dried, filtered and concentrated. The crude product was dissolved in DMF (15.5 ml). Cesium carbonate (4.00 g) and iodoacetamide (2.27 g) were added and the mixture was stirred at r.t. for 3 days. Water was added and the mixture was extracted with EtOAc. The org. phase was washed with water, dried, filtered and concentrated. The crude product was dissolved in MeOH and then concentrated to obtain a thick suspension. The solid was filtered off and washed with a small amount of MeOH. This procedure was repeated with the mother liquor to give (2-carbamoylmethoxy-4-cyano-benzyL)-carbamic acid tert-butyl ester (a total of 1.88 g) as a colorless solid. MS 304.2 ([M-HD The BOC protecting group of (2-carbamoylmethoxy-4-cyano-benzyl)-carbamic acid tert-butyl ester was removed using HC1 in dioxane to give 2-(2-aminomethyl-5-cyano-phenoxy)-acetamide hydrochloride as an off-white powder. MS 206.1 ([M+H]+)

The synthetic route of 144-48-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; F. HOFFMANN-LA ROCHE AG; WO2006/27135; (2006); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com