Month: August 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. 13918-92-8, name is 2,4-Difluorobenzene-1-sulfonyl chloride belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Safety of 2,4-Difluorobenzene-1-sulfonyl chloride

Intermediate 36: 2,4-Difluoro-N-(2-hydroxyethyl)-N-methyl-benzenesulfonamide 2,4-Difluorobenzenesulfonyl chloride (CAS no. 13918-92-8) (4.0 g, 19 mmol) in DCM (10 mL) was added slowly to a solution of 2-(methylamino)ethanol (1.66 mL, 20.7 mmol) in DCM (200 mL) and 10% sodium hydroxide solution (200 mL) at 0 C. The reaction was allowed to warm to room temperature and stirred for 20 hours. The DCM layer was separated and the aqueous re-extracted into DCM (2*50 mL). The combined organic extracts were washed with brine (200 mL), dried (MgSO4), filtered and evaporated under reduced pressure to afford the product (4.7 g, 98%). 1H NMR 6 (400 MHz, CDCl3): 1.98 (t, 1H), 2.94 (s, 3H), 3.32 (t, 2H), 3.79 (q, 2H), 6.94-7.03 (m, 2H), 7.89-7.95 (m, 1H).

The synthetic route of 13918-92-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; AstraZeneca AB; US2008/171734; (2008); 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. 202197-26-0, name is 3-Chloro-4-((3-fluorobenzyl)oxy)aniline belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Computed Properties of C13H11ClFNO

(I) Preparation of the compounds Example 1: Preparation of N-{4-[3-chloro-4-(3-fluoro-benzyloxy)phenylamino] quinazolin-6-yl}-acrylamide 3tep A: preparation of 4-[3-chloro-4-(3-fluoro-benzyloxy)phenylamino]-6-nitro-quinazoline 1.20 g (5.7 mmol) of 4-chloro-6-nitro-quinazoline (prepared by referring to WO 2007/082434) and 1.37 g (5.6 mmol) of 4-(3-fluoro-benzyloxy)-3-chloro-aniline (prepared by referring to WO 2007/082434) were dissolved in 80mL of isopropanol and refluxed for 3 hours. A large amount of yellow solid was precipitated from the system, and was filtered. The filter cake was washed with a saturated sodium bicarbonate aqueous solution till pH=8 and dried under vacuum to give 1.62g ( 3.75 mmol ) of yellow solid, which was identified as 4-[3-chloro-4-(3-fluoro-benzyloxy) phenylamino]-6-nitro-quinazoline with a yield of 67%. 1H-NMR (400MHz, CDCl3): delta 11.30(1H, br), 9.54-9.48(1H, m), 8.45-8.41(1H, m), 8.31-8.25(1H, m), 7.98-7.89(1H, m), 7.50-7.47(1H, m), 7.35-7.26 (1H, m), 7.05-6.96(1H, m), 6.90-6.80(2H, m), 7.74-7.60(2H, m), 4.84(2H, s).

The synthetic route of 202197-26-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Shanghai Allist Pharmaceuticals, Inc.; EP2292234; (2011); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 108-37-2,Some common heterocyclic compound, 108-37-2, name is 1-Bromo-3-chlorobenzene, molecular formula is C6H4BrCl, 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 i-butyl piperazine-l-carboxylate (1.96 g, 10.54 mmol, 2.00 equiv), 1- bromo-3-chlorobenzene (1 g, 5.26 mmol, 1.00 equiv), BINAP (330 mg, 0.53 mmol, 0.10 equiv), Pd2(dba)3 (243.8 mg, 0.27 mmol, 0.05 equiv), NaOi-Bu (1.59 g, 16.56 mmol, 3.00 equiv), and toluene (17 mL) was placed in a 100-mL round bottom flask, stirred overnight at 100C in an oil bath, and concentrated under vacuum. Purification via silica gel column (PE/EA (50:1)) yielded 1.3 g (83%) of i-butyl 4- (3-chlorophenyl)piperazine-l-carboxylate as a yellow solid. LC-MS (ES, m/z): 297 [M+H]+

The synthetic route of 108-37-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BIOENERGENIX; MCCALL, John, M.; MCKEARN, John; ROMERO, Donnal, L.; CLAIR, Michael; WO2011/28947; (2011); A2;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Synthetic Route of 139512-70-2, These common heterocyclic compound, 139512-70-2, name is 4-Chloro-5-fluorobenzene-1,2-diamine, 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: To a mixture of compound 11 (0.46 mmol) and appropriate o-phenylenediamines (0.46 mmol) in ethanol was added a solution of Na2S2O5 (770 mg, 4 mmol) in H2O (1.6 mL). The resulting mixture was stirred at reflux for 4 h. after completion of reaction; the solution was evaporated under reduced pressure to remove ethanol, and partitioned between EtOAc and water. The organic layer was dried over Na2SO4, and concentrated in vacuo. The crude product was purified by column chromatography using EtOAc/hexane as eluant to afford pure compounds 12(a-l) in good yields.

The synthetic route of 139512-70-2 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Kamal, Ahmed; Srinivasa Reddy; Polepalli, Sowjanya; Shalini, Nekkanti; Reddy, V. Ganga; Subba Rao; Jain, Nishant; Shankaraiah, Nagula; Bioorganic and Medicinal Chemistry; vol. 22; 19; (2014); p. 5466 – 5475;,
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. 7051-16-3, name is 1-Chloro-3,5-dimethoxybenzene, A new synthetic method of this compound is introduced below., Computed Properties of C8H9ClO2

General procedure: A 0.94 M soln of MeMgBr in THF (1.59 mL, 1.5 mmol) was added to a mixture of FeF3 (5.7 mg, 0.050 mmol) and 1,3-bis(2,6-diisopropylphenyl)imidazolinium chloride (64.4 mg, 0.15 mmol) in THF (2.0 mL) at 0C; 1-chloro-4-methoxybenzene (143 mg, 1.0 mmol) and undecane were then added at r.t. The mixture was stirred at 80 C for 24 h. The mixture was cooled to r.t. and an aliquot of the mixture was filtered through a Florisil pad. The product yield was determined by GC analysis (92% yield) using undecane as an internal standard. 1-Methoxy-4-methylbenzene is volatile, hence isolation was performed for the large-scale experiment using starting aryl chloride (5.6 mmol). The crude product was purified by column chromatography (silica gel, pentane, Rf = 0.06) and subsequent GPC to obtain the title compound (78.7 mg, 11%) as a colorless oil.

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; Agata, Ryosuke; Iwamoto, Takahiro; Nakagawa, Naohisa; Isozaki, Katsuhiro; Hatakeyama, Takuji; Takaya, Hikaru; Nakamura, Masaharu; Synthesis; vol. 47; 12; (2015); p. 1733 – 1740;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Synthetic Route of 13918-92-8, 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. 13918-92-8, name is 2,4-Difluorobenzene-1-sulfonyl chloride belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: To a stirred solution of 5-bromo-2-methoxypyridin-3-amine 1 (13.70 g, 67.5 mmol) in pyridine (140 mL) was added dropwise 2,4-difluorobenzenesulfonyl chloride 2 (14.35 g, 67.5 mmol) over 10 min at 0 C. The mixture, which quickly became heterogeneous, was allowed to warm to ambient temperature and stirred for 16 h, at which time the reaction was diluted with water (400 mL) and the solids were filtered and washed with water. The precipitate was dried in a vacuum oven at 60 C to give N-(5-bromo-2-methoxypyridin-3-yl)-2,4-difluorobenzenesulfonamide 3 (18.30 g, 71.3% yield) as a pale yellow powder, which was used without further purification.

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, 2,4-Difluorobenzene-1-sulfonyl chloride, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Han, Jinsong; Chen, Ying; Yang, Chao; Liu, Ting; Wang, Mingping; Xu, Haojie; Zhang, Ling; Zheng, Canhui; Song, Yunlong; Zhu, Ju; European Journal of Medicinal Chemistry; vol. 122; (2016); p. 684 – 701;,
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 6940-78-9 as follows. Computed Properties of C4H8BrCl

Add potassium carbonate (9.42 g) in water (10ml) in round bottom flask and stirred for 10-15 min at 30-35C. To this add DMF (50ml) and 7-Hydroxy quinolin-2(lH)-one (10g), heated the resulting mixture to 35-40C and stirred for 10-15 min. To this added 1-Bromo-4-chloro butane (21.29 g) and stirred the reaction mass for 6-8 hours at 35-40C, added water (20ml) drop wise over a period of 30-40 minutes and stirred the reaction mass for 30-40 min at 35-40C. Cooled the reaction mass to 10C, filtered and washed with methanol (20 ml) and DM water (20 ml) at 25-30C to obtain wet material. Yield: 11.0 g, HPLC purity- 95.8%; Dimer Impurity: 1.49% To the resulting wet material (11.0 g), methanol (200ml) was added at 25-30C and heated to reflux till complete dissolution. To this added AMBER LITE IR 120 H (10g) at 65-70C and stirred for 1-1.5 hours at reflux temperature. Filtered the resulting mixture through hyflo at 60-65C and cooled the filtrate to 5-10C and stirred for 30 minutes. Filtered the material, washed with methanol (10 ml) and dried at 60-65C for 5-8 hours. Yield: 8.0 g, HPLC purity: 97.3%; Dimer impurity: 0.027%.

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:
Patent; JUBILANT GENERICS LIMITED; BANSAL, Deepak; MISHRA, Himanchal; MISHRA, Vaibhav; SRIVASTAVA, Alka; VIR, Dharam; (24 pag.)WO2017/216661; (2017); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

These common heterocyclic compound, 2267-25-6, name is 2-Chloro-4-fluoroanisole, 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. Safety of 2-Chloro-4-fluoroanisole

2-Chloro-4-fluoro-1-methoxybenzene a8 (0.0160 g, 0.10 mmol), acridine photosensitizer (A) (0.0029 g, 0.005 mmol) and L-valine were added sequentially under argon atmosphere. Ethyl b1 (0.0218 g, 0.15 mmol), 1,2-dichloroethane (DCE) 2.0 mL.The reaction was irradiated for 48 hours under a 6W blue light at room temperature.After completion of the reaction, the solvent was evaporated under reduced pressure and purified by column chromatography, eluting solvent: (V) petroleum ether / (V) ethyl acetate = 20/1.A yellow liquid (25) (0.0191 g, 87%) was obtained.

The synthetic route of 2-Chloro-4-fluoroanisole has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Central China Normal University; Zhou Shaolin; Shi Weimin; (27 pag.)CN110294685; (2019); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Electric Literature of 328-84-7, These common heterocyclic compound, 328-84-7, name is 3,4-Dichlorobenzotrifluoride, 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.

The procedure of Example 4 was repeated but using 3,4-dichlorobenzotrifluoride. After work up there was isolated a 95% yield of the title compound. It was shown that 100% of the starting material had been consumed, thus indicating that the reaction had occurred with both high selectivity and high yield.

Statistics shows that 3,4-Dichlorobenzotrifluoride is playing an increasingly important role. we look forward to future research findings about 328-84-7.

Reference:
Patent; Aventis CropScience, S.A.; US6410737; (2002); B1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Reference of 14752-66-0, 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. 14752-66-0, name is Sodium 4-chlorobenzenesulfinate, This compound has unique chemical properties. The synthetic route is as follows.

A method for preparing a distyryl sulfide compound, comprising the steps of:0.3mmol (0.0541g)1,1-stilbene, 0.45 mmol (0.0894 g) of sodium p-chlorobenzenesulfinate and 0.2558 g of a 45% by mass aqueous solution of hydroiodic acid (containing 0.9 mmol of hydroiodic acid) were dispersed in 2 mL of toluene. The coupling reaction was carried out at 75 C for 15 h, quenched with a saturated aqueous solution of sodium thiosulfate, and extracted with dichloromethane (15 mL×3).The liquid layer was separated, and the organic layer was dried over anhydrous sodium sulfate.Dry under reduced pressure, and the column was passed to give 0.0812 g of distyryl thioether compound (white solid, yield 84%)

The chemical industry reduces the impact on the environment during synthesis Sodium 4-chlorobenzenesulfinate. I believe this compound will play a more active role in future production and life.

Reference:
Patent; South China Normal University; Guangdong Pharmaceutical University; Wang Chaoyang; Wang Bowen; Zou Bo; Zhan Haiying; (17 pag.)CN110305051; (2019); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics