Category: chlorides-buliding-blocks

Synthetic Route of 622-24-2,Some common heterocyclic compound, 622-24-2, name is (2-Chloroethyl)benzene, molecular formula is C8H9Cl, 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.

3-Ethyl-4-methyl-2-oxo-3-pyrroline-1-carboxamide (A) (35 g, 2.1 mol) and (2-chloroethyl)benzene (B) (32.8 g, Mix 2.52 mol) and add 50% sodium hydroxide solution (55ml),In a flask of a mixture of petroleum ether (72 ml) and copper iodide (5.07 g, 0.78 mol), the reaction was carried out at 85C for 9 hours. After the reaction was completed, the temperature was lowered to 6C to obtain of 3-ethyl-4-methyl-2-oxo-N-(2-phenylethyl)-2,5-dihydro-1H-pyrrole-1-carboxamide (C) (53.8 g) in a yield of 85.24%.Purity is 99.78%.

The synthetic route of 622-24-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Dong Dandan; (7 pag.)CN107963988; (2018); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Electric Literature of 33863-76-2, These common heterocyclic compound, 33863-76-2, name is 1-Bromo-3-chloro-5-fluorobenzene, 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.

Example 21Synthesis of {3-Chloro-5-[4-(2,2-dimethyl-propionylamino)-2-(2,2,2-trifluoro-ethylsulfanylmethyl)-phenoxy]-phenyl}-acetic acid (Compound 28) cl Step 1: 1-Benzyloxy-3-bromo-5-chloro-benzene; To 1-bromo-3-chloro-5-fluorobenzene (25 g, 112 mmol) and benzyl alcohol (25 mL, 239 mmol) in NMP (200 mL) at room temperature was added sodium hydride (60% in mineral oil; 10.5 g, 263 mmol), and the reaction was heated to 120 C. for 10 hours. The mixture was acidified with 10% aqueous HCl and extracted with EtOAc to give the title compound.

The synthetic route of 33863-76-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; AMIRA PHARMACEUTICALS, INC.; US2010/4331; (2010); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

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. 29671-92-9, name is Carbamimidic chloride hydrochloride belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. category: chlorides-buliding-blocks

Step 3; 2-Amino-6- (4-chloro-2-methylphenoxymethyl)benzonitrile mg; 0.29 mmol) and chloroformamidine hydrochloride (51.0 mg, 0.44 mmol) were heated at 140 C in diglyme for 3 hours. The reaction mixture was diluted with water, stirred for 2 hours, filtered, washed with water and dried. Purification by silica gel chromatography (5% methanol in dichloromethane) yielded 55 mg of the 5-(4-chloro- 2-methylphenoxymethyl) quinazoline-2,4-diamine.

The synthetic route of 29671-92-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; DECODE CHEMISTRY, INC.; SINGH, Jasbir; GURNEY, Mark E.; WO2005/123724; (2005); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

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 16799-05-6 as follows. Product Details of 16799-05-6

The reaction bottle by adding 0.5 millimoles of 2 – phenyl indole, 1.0 mmol 3 – chlorobenzene ethyl alkyne bromine, 3 mmol (6 equiv) potassium hydroxide, 5 muM % (0.025mmol) Pd (OAc)2, 15 muM % (0.075mmol) PCy3, 1.5 ml of N, N – dimethyl formamide, under nitrogen conditions, 130 C stirring for 18 hours, stop heating and stirring, cooled to the room temperature, distilled under reduced pressure to get the crude product, through the column chromatography separation and purification, to obtain the target product, the used column chromatography eluant is petroleum ether, yield 65%. This embodiment of the obtained product hydrogen spectrogram and carbon spectrogram as shown in Figure 11, Figure 12 is shown

According to the analysis of related databases, 16799-05-6, the application of this compound in the production field has become more and more popular.

Reference:
Patent; South China University of Technology; Wu Wanqing; An Yanni; Li Jianxiao; Jiang Huanfeng; (16 pag.)CN106866664; (2017); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 83121-15-7, The chemical industry reduces the impact on the environment during synthesis 83121-15-7, name is 3,5-Dichloro-2,4-difluoroaniline, I believe this compound will play a more active role in future production and life.

In a 500ml stainless steel autoclave equipped with a hydrogen port, cooling circulating water, pressure gauge and electric heating device,160 g of methanol and 22.8 g (0.1 mol) of compound (II) 3,5-dichloro-2,4-difluoronitrobenzene were added.0.80 g of 3% platinum carbon and 0.85 g (0.007 mol) of 85% phosphoric acid were added by stirring, and the pipe was rinsed with 20 g of methanol to close the kettle;Wherein the molar amount of platinum carbon is calculated as 0.80*(1-60% aqueous)*3% dry basis platinum content/195.078 platinum molecular weight=0.0000492 mol; First, hydrogen is introduced to the internal pressure of 0.2 to 0.4 MPa for 2 to 3 times, then hydrogen is introduced to the internal pressure of 1.0 to 1.5 MPa, and the temperature is controlled at 75 to 80 C to stir the reaction. During the period, hydrogen is added until the pressure is no longer lowered.HPLC monitoring raw material (II) basically disappeared or the content was less than 0.5%; reaction 6h, the reaction solution was suction filtered, the filter residue was washed twice with methanol, 10ml each time; solid platinum carbon was recovered and applied; The filtrate was vacuum-recovered to recover a large amount of light yellow solids. The mixture was stirred and dripped into 50 g of water, stirred rapidly for 30 minutes, slowly cooled to 0 to 5 C for 1 h, filtered, and dried.The solid was further washed with water to neutrality, rinsed with 10 g of water, and dried at 50 C under normal pressure to obtain a white-white powdery solid. The weight: 19.0 g, content: 97.2%; yield: 96.0%.

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, 3,5-Dichloro-2,4-difluoroaniline, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Jiangsu Zhongqi Technology Co., Ltd.; Chen Qinghong; Zhang Pu; Wang Fengyun; Hou Yuanchang; (7 pag.)CN109369414; (2019); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

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. 6940-78-9, name is 1-Bromo-4-chlorobutane, This compound has unique chemical properties. The synthetic route is as follows., COA of Formula: C4H8BrCl

General procedure: A 2.6 M methanolic solution of MeSNa (23 mL, 1.2 equiv.) was added dropwise to a stirred solution of omega-bromochloroalkane 6 (50 mmol) in dry methanol (80 mL) at room temperature (r.t.). Stirring was continued until complete consumption of the dihalide (2-3 h, GC monitoring). The mixture was concentrated in vacuo and the resulting white slurry was taken in cold water and extracted with dichloromethane. After drying the organic phase over MgSO4, filtration and concentration in vacuo, the oily residue was purified by flash chromatography using silica gel (230-400 mesh) with hexane as eluent to afford 7a-d as light yellow oils.

According to the analysis of related databases, 6940-78-9, the application of this compound in the production field has become more and more popular.

Reference:
Article; Mavratzotis, Manolis; Cassel, Stephanie; Montaut, Sabine; Rollin, Patrick; Molecules; vol. 23; 4; (2018);,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 1996-30-1, name is 3-Bromo-4-fluorochlorobenzene, belongs to chlorides-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 1996-30-1, SDS of cas: 1996-30-1

A solution of 2-bromo-4-chloro-l-fluorobenzene (2.5 mL, 20 mmol) and sodium thiomethoxide (1.45 g, 20.7 mmol) in DMF (20 mL) was stirred at 100C for 2 h. The reaction mixture was added to water (20 mL) with stirring, and the aqueous mixture was extracted with ethyl acetate (3 x 50 mL). The combined organic layers were dried over sodium sulfate, filtered and concentrated in vacuo. The residue was purified by column chromatography on silica gel(hexanes/EtOAc: 20/1) to afford the title compound. 1H NMR (600 MHz, DMSO-d6): delta 7.74 (d, / = 8.6, 2.3 Hz, 1H), 7.49 (dd, / = 8.6, 2.3 Hz, 1H), 7.28 (d, / = 8.6 Hz, 1H), 2.51 (m, 3H).

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-Bromo-4-fluorochlorobenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; MERCK SHARP & DOHME CORP.; CHILDERS, Matthew Lloyd; DINSMORE, Christopher; FULLER, Peter; GUERIN, David; KATZ, Jason David; PU, Qinglin; SCOTT, Mark E.; THOMPSON, Christopher F.; ZHANG, Hongjun; FALCONE, Danielle; TORRES, Luis; BRUBAKER, Jason; ZENG, Hongbo; CAI, Jiaqiang; DU, Xiaoxing; WANG, Chonggang; BAI, Yunfeng; KONG, Norman; LIU, Yumei; ZHENG, Zhixiang; WO2014/146490; (2014); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 1000572-93-9, name is 1-Bromo-3,4-dichloro-5-fluorobenzene, belongs to chlorides-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 1000572-93-9, Safety of 1-Bromo-3,4-dichloro-5-fluorobenzene

A mixture of 5-bromo-1,2-dichloro-3-fluorobenzene (2 g, 8.3 mmol), bis(pinacolato)diboron (3.1 g, 12.4 mmol), Pd(dppf)Cl2 (0.33 g, 0.41 mmol), KOAc (2.4 g, 24.7 mmol) in 1,4-dioxane (50 mL) was degassed with N2 for 5 minutes. The reaction mixture was stirred at 70 C. for 16 h. TLC (EtOAc/Petroleum ether=1:5) indicated complete consumption of the bromo starting material. The reaction mixture was poured into water (40 mL) and extracted with EtOAc (3*70 mL). The combined organic phases were dried over anhydrous Na2SO4, and concentrated in vacuo to give a crude residue, which was purified by column chromatography (silica gel, EtOAc/petroleum ether=1:10) to give the boron intermediate (2.0 g, yield: 83.3%) as a white solid.

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; Anacor Pharmaceuticals, Inc.; Eli Lilly and Company; Akama, Tsutomu; Balko, Terry William; Defauw, Jean Marie; Plattner, Jacob J.; White, William Hunter; Winkle, Joseph Raymond; Zhang, Yong-Kang; Zhou, Yasheen; US2013/131016; (2013); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Synthetic Route of 4535-90-4,Some common heterocyclic compound, 4535-90-4, name is 2-Chloro-N-methylethanamine hydrochloride, molecular formula is C3H9Cl2N, 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 solution of 50 mg of 3-((2-(4-((3-(trifluoromethyl)benzyl)carbamoyl)pyridin-2-yl)-4-(piperidin-1-yl)phenyl)carbamoyl)benzoic acid 4.1e, 9.3 mg of N-methyl-N-(2-chloroethyl)amine hydrochloride, 43 muL of diisopropylethylamine, and 35 mg of HATU in 1000 muL of DMF was stirred for 1 h. The mixture was diluted with 20 mL of water, and the resulting precipitate was collected by filtration. It was dissolved in dichloromethane and the solution was washed with water and dried (Na2SO4). The solvent was evaporated to give 42 mg of product.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2-Chloro-N-methylethanamine hydrochloride, its application will become more common.

Reference:
Patent; Ardelyx, Inc.; Lewis, Jason G.; Jacobs, Jeffrey W.; Reich, Nicholas; Leadbetter, Michael R.; Bell, Noah; Chang, Han-Ting; Chen, Tao; Navre, Marc; Charmot, Dominique; Carreras, Christopher; Labonte, Eric; (323 pag.)US9301951; (2016); B2;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

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. 32768-54-0, name is 2,3-Dichlorotoluene, A new synthetic method of this compound is introduced below., HPLC of Formula: C7H6Cl2

EXAMPLE 1 Preparation of 2,3-dichloro-6-nitrotoluene 208 mmole concentrated nitric acid and 270 mmole concentrated sulfuric acid were mixed and cooled to ambient temperature. 200 mmole 2,3-dichlorotoluene was added to a reaction flask and was cooled in an ice-water bath. The acid mixture was added slowly with stirring to the dichlorotoluene keeping the dichlorotoluene in the ice-water bath. After all the acid had been added, the mixture in the ice-water bath was stirred for about 10 minutes. A drying tube was attached to the reaction flask and the reaction mixture warmed to ambient temperature. The reaction mixture was heated at 50 C. with stirring for three hours. The reaction mixture was transferred to a separatory funnel and the acid drained. The organic layer was washed with water and discarded. 1 % sodium carbonate was added to neutralize the acid. Ethyl acetate was added and partitioned the product to the organic phase. Ethyl acetate was added until the organic phase cleared. The organic phase was washed with water, followed by washing with half-saturated aqueous brine solution and washing with saturated aqueous brine solution. The organic phase was dried with sodium sulfate and the solvent evaporated under reduced pressure. The crude product was purified by flash column chromatography using silica gel 60 (35 to 70-um particle size) at 5% product loading. The elution solvent was 100% hexane. Unreacted starting material elutes first followed by the ortho nitro product then by a material hypothesized to be the para nitro compounds. The yield was about 50% of a light yellow solid based on 2,3-dichlorotoluene.

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:
Patent; Roberts Laboratories Inc.; US5801245; (1998); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics