Tag: M.W=200-300

Some common heterocyclic compound, 460-37-7, name is 1,1,1-Trifluoro-3-iodopropane, molecular formula is C3H4F3I, 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: 460-37-7

2.0 g (9:51 mmol) of the compound from Ex. 164A and 3.29 g (23.8 mmol) of potassium carbonate were stirred in 50 ml of anhydrous DMF for 15 min at RT before 3.3 ml (28.5 mmol) 1,1,1-trifluoro-3-iodopropane have been added .Since the conversion was not complete after stirring overnight at RT , further 1.39 g (9:51 mmol) of potassium carbonate with 1.1 ml (9.51 mmol) of 1,1,1-trifluoro-3-iodopropane are added and the mixture was heated for 2 h at 60 C .After cooling to RT was diluted with ethyl acetate and washed successively twice with water and once with saturated sodium chloride solution.After drying over anhydrous magnesium sulfate, was filtered and the filtrate concentrated to dryness.The crude product was purified by chromatography on a silica gel cartridge (Biotage, 340 g silica gel, eluent: cyclohexane / ethyl acetate 24: 1 -> 10: 1).After concentration and drying of the product fractions 2:06 g (70% d. Th.) Of the title compound.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 460-37-7, its application will become more common.

Reference:
Patent; BAYER PHARMA AKTIENGESELLSCHAFT; HAERTER, MICHAEL; DELBECK, MARTINA; KALTHOF, BERND; LUSTIG, KLEMENS; LINDNER, NIELS; KAST, RAIMUND; WASNAIRE, PIERRE; SUESSMEIER, FRANK; (372 pag.)TW2016/7950; (2016); A;,
Iodide – Wikipedia,
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Some common heterocyclic compound, 64248-58-4, name is 1,2-Difluoro-4-iodobenzene, molecular formula is C6H3F2I, 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. name: 1,2-Difluoro-4-iodobenzene

A mixture of methyl indole-5-carboxylate Ij (2 g, 11.4 mmol), l-iodo-3,4-difluoro-benzene Io (1.5 mL, 12.5 mmol), CuI (0.22 g, 1.14 mmol), trans-N, N’-dimethylcyclohexane-l,2- diamine (0.54 mL, 3.43 mmol), and K3PO4 (6.06 g, 28.5 mmol) in toluene (12 mL) was heated at 110 0C for 7 hours. The reaction mixture was diluted with CH2CI2 and filtered. The solution was concentrated and the residue was purified by flash column chromatography (silica gel, 20% EtOAc/heptane) to give Ip (3.0 g).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 64248-58-4, its application will become more common.

Reference:
Patent; JANSSEN PHARMACEUTICA NV; BIAN, Haiyan; CHEVALIER, Kristen, M.; CONNOLLY, Peter, J.; FLORES, Christopher, M.; LIN, Shu-chen; LIU, Li; MABUS, John; MACIELAG, Mark, J.; MCDONNELL, Mark, E.; PITIS, Philip, M.; ZHANG, Sui-po; ZHANG, Yue-mei; ZHU, Bin; CLEMENTE, Jose; WO2010/124082; (2010); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 627-31-6, 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. 627-31-6, name is 1,3-Diiodopropane(stabilized with Copper chip), This compound has unique chemical properties. The synthetic route is as follows.

Example 7; [0055] Synthesis of 3-(benzyloxy)-1 -(3-iodopropyl)pyridin-2(1 H)-one(Compound 7); To a solution of 1 ,3-diiodopropane (7.1 ml_, 63 mmol) in tetrahydrofuran (50 ml_) was added 3-(benzyloxy)pyhdin-2(1 H)-one (1.28 g, 6.3 mmol) and Na2CO3 (0.67 g, 6.3 mmol). The mixture was then stirred at 70 0C for 1 day. Reaction progress was monitored by ES-MS. After ESMS showed essentially complete consumption of the starting material 3-(benzyloxy)pyhdin-2(1 H)-one, the reaction was stopped. Then the reaction mixture was filtered, concentrated, and subjected to flash column chromatography (eluent: hexane : ethylacetate 1 :1 ). Compound 7 was obtained (240 mg, 10% yield). Analysis: ES-MS (positive ion in MeOH/H2O): m/z = 370.2, ([M+H]+, calculated: 370.03).

The chemical industry reduces the impact on the environment during synthesis 1,3-Diiodopropane(stabilized with Copper chip). I believe this compound will play a more active role in future production and life.

Reference:
Patent; BOARD OF SUPERVISORS OF LOUISIANA STATE UNIVERSITY AND ARGRICULTURAL AND MECHANICAL COLLEGE; WO2008/100907; (2008); A2;,
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. 29289-13-2, name is 2-Iodo-4-methylaniline, This compound has unique chemical properties. The synthetic route is as follows., Application In Synthesis of 2-Iodo-4-methylaniline

General procedure: A mixture of 2-iodoaniline 1 (1 mmol), benzylamine 2 (1.2 mmol), sulfur powder (6 mmol), DABCO (2 mmol), Cu(OAc)2.H2O (0.02 mmol), and 1,10-phenanthroline (0.02 mmol) was stirredin DMSO (5 mL) at 100 C. After completion of the reaction as indicated by TLC, the mixture was cooled to room temperature, water (20 mL) was added, and then the aqueous solution was extracted with ethyl acetate (3 15 mL). The organic layers were combined, dried over anhydrous MgSO4, the filtrate was concentrated under vacuum and then the residue was purified by column chromatography (eluent: petroleum ether/ethyl acetate (10:1 to 14:1) on silicagel to provide the desired product.

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 29289-13-2.

Reference:
Article; Wang, Rui; Ding, Yong-Liang; Liu, Hong; Peng, Shu; Ren, Jie; Li, Lei; Tetrahedron Letters; vol. 55; 4; (2015); p. 945 – 949;,
Iodide – Wikipedia,
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Adding a certain compound to certain chemical reactions, such as: 156150-67-3, name is 2-Chloro-1-fluoro-4-iodobenzene, 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 156150-67-3, Product Details of 156150-67-3

Intermediate 5: Ethyl 1-(3-chloro-4-fluorophenyl)-5-methyl-1 H-1 ,2,3-triazole-4- carboxylate; To a mixture of 2-chloro-1-fluoro-4-iodobenzene (0.5 g, 1.950 mmol) and ethyl 2- butynoate (0.227 ml, 1.950 mmol) in water/DMSO (0.22ml/2ml) at room temperature was added L-proline (0.045 g, 0.390 mmol), sodium carbonate (0.041 g, 0.390 mmol), sodium azide (0.152 g, 2.340 mmol), sodium l-ascorbate (0.039 g, 0.195 mmol) and copper(ll) sulfate pentahydrate (0.024 g, 0.097 mmol) (in this order) and the mixture was heated at 65 0C overnight. On cooling to room temperature, the mixture was quenched with aqueous ammonia (1 ml) and EtOAc (20ml) and water (20 ml) were added. The two phases were separated, and the aqueous phase was extracted with EtOAc (3 x 30 ml). All organic phases were combined and washed with water/brine (50ml) repeatedly. The organic phase was dried over sodium sulfate, filtered and the solvent was evaporated to afford a crude product that was purified by MDAP to afford the title compound (6.5%); MH+=284.

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

Reference:
Patent; GLAXO GROUP LIMITED; WO2009/115486; (2009); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 52914-23-5, These common heterocyclic compound, 52914-23-5, name is 2-(4-Iodophenyl)ethanol, 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.

A mixture of 1.14 g (4.60 mmol) of 2-(4-iodophenyl)ethanol, 0.88 g (6.89 mmol) of 4-chlorophenol, 2.99 g (9.20 mmol) of cesium carbonate, 0.14 g (1.38 mmol) of N,N-dimethylglycine and 0.087 g (0.46 mmol) of cuprous iodide in 4 ml of dioxane is heated at 90 C. for 24 hours with thorough stirring under an argon atmosphere. It is cooled to ambient temperature and taken up in 150 ml of ethyl acetate and 50 ml of water. After the phases have settled and been separated, the organic phase is washed with 25 ml of water and 25 ml of saturated aqueous sodium chloride solution, dried over magnesium sulphate and evaporated to dryness. The residue is purified by chromatography on silica gel, eluting with an 85/15 then 75/25 mixture of cyclohexane and ethyl acetate, to give 0.68 g of product in the form of an oil.

The synthetic route of 52914-23-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Sanofi-Aventis; US2006/14830; (2006); A1;,
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. 104539-21-1, name is 1-Iodo-2-(2-methoxyethoxy)ethane, This compound has unique chemical properties. The synthetic route is as follows., category: iodides-buliding-blocks

The 20 g of the above-mentioned synthesis of diethylene glycol monomethyl ether halogenated compounds and 10 ml 1 – methyl imidazole is added to the 50 ml flask, 80 C magnetic stirring reaction 60 h. After the reacting liquid to return to room temperature, ethyl acetate to fully wash, liquid orange viscous liquid obtained after, and in 120 C vacuum dried to obtain 1 – methyl -3 – diethylene glycol monomethyl ether imidazole iodide, is put into the glove box in standby.

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 104539-21-1.

Reference:
Patent; Dalian Institute of Chemical Physics; Sun Gongquan; Yang Congrong; Wang Suli; (11 pag.)CN108218782; (2018); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 444-29-1, The chemical industry reduces the impact on the environment during synthesis 444-29-1, name is 1-Iodo-2-(trifluoromethyl)benzene, I believe this compound will play a more active role in future production and life.

General procedure: A 10 mL flask equipped with a Teflon valve was charged with a magnetic stir bar, CuI (2 mg, 1molpercent), Heteroarylamine (1.5 mmol), KOtBu (224 mg, 2.0 mmol), solid aryl halides (1.0 mmol). The tube was evacuated and backfilled with argon. Under a counter flow of argon, dioxane (1.5mL), aryl halides (1.0 mmol, if liquid) were added by syringe. The tube was sealed. The reaction mixture was allowed to stir at 110 °C (X=I) or 130 °C (X= Br) for 24 h. Then the mixture was cooled to room temperature and added 5.0 mL brine. Subsequently, the mixture was extracted with ethyl acetate. The organic layers were collected, dried over Na2SO4, filtered and the solvent was removed under vacuum. The residue was purified by column chromatography on silica gel.

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, 1-Iodo-2-(trifluoromethyl)benzene, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Wang, Deping; Kuang, Daizhi; Zhang, Fuxing; Liu, Yang; Ning, Shunhua; Tetrahedron Letters; vol. 55; 51; (2014); p. 7121 – 7123;,
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. 82998-57-0, name is 3-Iodo-4-methylbenzoic acid, This compound has unique chemical properties. The synthetic route is as follows., SDS of cas: 82998-57-0

INTERMEDIATE 8; [2-methyl-5-(5-methyl-1 ,3,4-oxadiaz -2-yl)phenyl]boronic acid; a) Methyl 3-iodo-4-methylbenzoate; A suspension of 3-iodo-4-methylbenzoic acid (15.00 g, 60.00 mmol) and a 4M solution of hydrochloric acid in dioxane (20.00 mL, 80.0 mmol) in methanol (20 mL) was heated in a sealed tube at 80 C with stirring. After stirring for 3 days, the mixture was cooled and ethyl acetate and saturated aqueous potassium carbonate solution were added. The organic layer was washed with brine, dried (MgS04) and evaporated in vacuo to give the title compound (15.00 g, 95%).LR S (m/z): 277 (M+1)+.

According to the analysis of related databases, 82998-57-0, the application of this compound in the production field has become more and more popular.

Reference:
Patent; ALMIRALL, S.A.; AIGUADE BOSCH, Jose; CARRANCO MORUNO, Ines; WO2011/57757; (2011); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 52548-14-8,Some common heterocyclic compound, 52548-14-8, name is 2-Iodo-5-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.

Add 1.1 kg of acetone to the 5L reaction flask.131g 2-iodo-5-methylbenzoic acid,Stir and dissolve,Add 350g of anhydrous potassium carbonate,After heating to reflux (55-60 C) for half an hour, add 114g 1,2,3-triazole,2.4 g of cuprous iodide.The reaction was kept under reflux (55-60 C) for 8 hours, sampled, and sampled once every 1 h. After the reaction was completed, it was cooled to room temperature for filtration, and the filter cake was washed twice with 120 g of acetone to obtain a white solid at room temperature (20-30 C). The white solid was dissolved in 1.3 kg of purified water and stirred.After 30 min, hydrochloric acid was added dropwise at room temperature to adjust the pH of the system to 1.5-2.0 to obtain a large amount of white solid. It was stirred for 1-2 hours, filtered, and the filter cake was washed twice with purified water. The resulting solid was dried to dryness at 50 ± 5 C to give a crude compound.Add 1 compound of crude product, 0.2 kg of absolute ethanol and 0 kg of purified water to a 1 L reaction flask, and warm to 75-80 C.Clear, heat for half an hour, cool to 0-5 C, filter, filter cake with a cold ethanol solution rinse, to obtain a white solid compound 1 boutique.The compound 1 was placed in a blast drying oven at a temperature of 55 C ± 5 C and dried for 5 h. Sampling, sampling every 2h 1Time, until the test (rapid moisture analyzer: 105 C, 10 min) loss on drying ? 0.5%, get Suwoleisheng intermediate products -Compound 1 was fine white crystalline solid 86 g, yield: 93%. Purity: 99.91%, Cu < 5 ppm. The synthetic route of 52548-14-8 has been constantly updated, and we look forward to future research findings. Reference:
Patent; Yangzijiang Pharmaceutical Group Co., Ltd.; Zou Yiquan; Xu Jingren; Cai Wei; Xuan Jingan; Chen Lingwu; Ji Ye; Zhu Yunlong; Liu Jinfeng; Hu Tao; (8 pag.)CN109810067; (2019); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com