Author: tianli

Related Products of 13918-92-8, 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. 13918-92-8 name is 2,4-Difluorobenzene-1-sulfonyl chloride, 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.

A mixture of 75 mg (0.22 mmol) E-7, 59 mu. (0.44 mmol) 2,4-difluoro-benzenesulfonyl chloride and 56 mu. (0.71 mmol) pyridine in 3 mL DCM is stirred over night at RT. The reaction mixture is concentrated under reduced pressure and the residue is purified by RP chromatography (C18, 20-90% acetonitrile in water containing 0.1% formic acid). Yield: 52 mg (46%). HPLC-MS: M+H = 516; tR = 1, 17 min.

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

Reference:
Patent; BOEHRINGER INGELHEIM INTERNATIONAL GMBH; WUNBERG, Tobias; VEEN, Van Der, Lars; KRAEMER, Oliver; WO2012/101186; (2012); A1;,
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. 14752-66-0, name is Sodium 4-chlorobenzenesulfinate, This compound has unique chemical properties. The synthetic route is as follows., HPLC of Formula: C6H4ClNaO2S

General procedure: Pyrazoles 4 (0.5 mmol), sodium sulfinate 2 (1.0 mmol) and NBS or NIS (1.5 mmol) were dissolved in 2 mL of EtOAc solvent. the reaction mixture was stirred at room temperature under air for 12 h. After the reaction, the resulting mixture was extracted with EtOAc. The combined organic phase was dried over anhydrous Na2SO4 and the solvent was then removed under vacuum. The residue was purified by flash column chromatography on silica gel (petroleum ether/ethyl acetate, 3:1) to afford the corresponding 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 14752-66-0.

Reference:
Article; Fu, Lili; Bao, Xiaodong; Li, Shanshan; Wang, Lingtian; Liu, Zhiguo; Chen, Wanzhi; Xia, Qinqin; Liang, Guang; Tetrahedron; vol. 73; 17; (2017); p. 2504 – 2511;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

32768-54-0, name is 2,3-Dichlorotoluene, belongs to chlorides-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. COA of Formula: C7H6Cl2

Example 14 endo-8-(2-Chloro-3-methyl-4-nitrophenyl)-8-azabicyclo[3.2.1]octan-3-ol (196MBT14-B) To a suspension of 2,3-dichlorotoluene (500 mg, 3.11 mmol) in concentrated sulfuric acid (2.5 mL) was added dropwise a solution of potassium nitrate (314 mg, 3.11 mmol) in concentrated sulfuric acid (2.5 mL) at room temperature. The resulting suspension was stirred 1 hour at room temperature and then poured into ice/water (100 mL) under stirring. The resulting aqueous phase was basified to pH 10 by addition of 25% aqueous ammonia and subsequently extracted with dichloromethane (2¡Á100 mL). The combined organic phases were dried over sodium sulphate, filtered and evaporated. The crude product was purified by preparative TLC (0-100% ethyl acetate in heptane) to give a 4:1 mixture of 6- and 5-nitrated product (232 mg). 80 mg of this mixture was dissolved in pyridine (1 mL). Nortropine (198 mg, 1.553 mmol) was added and the mixture was heated to 110 C. in a sealed flask for 20 hours and then concentrated. The residue was dissolved in 2 M HCl (20 mL) and extracted with dichloromethane (2¡Á20 mL). The combined organic phases were dried over Na2SO4, filtered and evaporated, and the resulting oil was purified by preparative TLC (eluting with dichloromethane) to afford the title compound (35 mg, 14% from 2,3-dichlorotoluene) as a yellow solid. LC/MS m/z 297 [M+H]+. 1H-NMR (CDCl3) delta 7.76 (d, J=10.5, 1H), 6.80 (d, J=10.5, 1H), 4.24-4.16 (m, 1H), 4.14-4.05 (m, 2H), 2.59 (s, 3H), 2.40-2.25 (m, 4H), 1.97-1.81 (m, 4H), 1.55 (s, 1H).

The synthetic route of 32768-54-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Schlienger, Nathalie; Thygesen, Mikkel Boas; Pawlas, Jan; Badalassi, Fabrizio; Lewinsky, Rasmus; Lund, Birgitte Winther; Olsson, Roger; US2006/160845; (2006); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Synthetic Route of 20850-43-5, These common heterocyclic compound, 20850-43-5, name is 5-(Chloromethyl)benzo[d][1,3]dioxole, 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.

Preparation of compound Ig: 2-(Benzo[l,3]dioxol-5-ylmethyl-methyI-amino)-ethanol. 2-(Methylamino)ethanol (22.0 g, 290 mmol) was added to a stirred solution of 3,4- methylenedioxybenzyl chloride (25.0 g, 147 mmol) in DCM (45 mL) at -780C under nitrogen. The solution was stirred for 15 minutes at -78 0C then warmed to room temperature and stirred for 16h. 1.2 M NaOH (100 mL) was added and the phases were separated. The organic layer was washed water (2 x 150 mL) and concentrated under vacuum to give 25.3 g (83%) of 2-(benzo[l,3]dioxol-5-ylmethyl- methyl-amino)-ethanol as a clear oil.

Statistics shows that 5-(Chloromethyl)benzo[d][1,3]dioxole is playing an increasingly important role. we look forward to future research findings about 20850-43-5.

Reference:
Patent; KALYPSYS, INC.; WO2007/62410; (2007); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Some common heterocyclic compound, 2106-02-7, name is 2-Chloro-4-fluoroaniline, molecular formula is C6H5ClFN, 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. SDS of cas: 2106-02-7

General procedure: The synthesis of azides were carried out according to the publish procedure [59]. Briefly, aniline (1eq) was dissolved in6N HCl solution (10mL/mmol of aniline) at room temperature and cooled up to 0C, followed by addition of aqueous NaNO2 (1eq) solution under stirring. After 10min of stirring at same temperature, sodium azide (1.2eq) was added to the reaction mixture. This mixture was further stirred at room temperature for 2-3h. The reaction was worked up by extraction with chloroform. The organic layer was washed with brine solution and dried over Na2SO4. After evaporation of the solvent, the crude product (3a-r) was pure enough for further reactions. All the synthesized azides were stored at-20C.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2106-02-7, its application will become more common.

Reference:
Article; Kant, Rama; Singh, Vishal; Nath, Gopal; Awasthi, Satish Kumar; Agarwal, Alka; European Journal of Medicinal Chemistry; vol. 124; (2016); p. 218 – 228;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Electric Literature of 6940-78-9, The chemical industry reduces the impact on the environment during synthesis 6940-78-9, name is 1-Bromo-4-chlorobutane, I believe this compound will play a more active role in future production and life.

Example 47:7 – hydroxy – 250 ml 111H-quin -2 – ketone (8.06g, unitunitunitant ), potassium carbonate (0.05 muM, unitunitunitant 0.075 muM), N, N’ – 50 ml dimethylacetamide), N, N?-dimethylformamido 40 C), and 7.95g bromo 10 min-chlorobutane (10.29g 1 – 0.06 muM, unitunitunits -4 -) were added to the unitunito-type reaction flask. Unitunitaceous . 50 C was stirred under the unitunitaceous 5 hours conditions. After completion of the reaction, water is quenched, solid precipitated, filtered, washed, and the solid obtained is recrystallized, obtaining 7 – (4 – polychloroprene) – 111H-quinoline -2 – ketone 11.8g, 93.7% and gave a Kunit, and a 98.5% purity Kunitz . Example 47 of data characterization: 7 – (4 – Chlorphenoxy) – 111H-quinolin -2 -one prepared.

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

Reference:
Patent; Zhejiang University of Technology; Weng Yiyi; Yang Ting; (25 pag.)CN109970705; (2019); A;,
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. 54932-72-8, name is 4-Bromo-1-chloro-2-methylbenzene, A new synthetic method of this compound is introduced below., Safety of 4-Bromo-1-chloro-2-methylbenzene

To a stirring solution of 4-bromo-1-chloro-2-methyl-benzene 5 (4.92mL, 37.1mmol) in THF (75mL) cooled to -78C was added n-butyllithium (14.9mL, 37.1mmol) dropwise. The solution was stirred at -78C for 30min and then was added to a stirring solution of phthalic anhydride 6 (5.00g, 33.8mmol) in THF (90mL) at -78C. The reaction was stirred at -78C for 2h before being quenched with 1N HCl (100mL). The solution was allowed to warm to rt, the layers were separated and the aqueous layer was extracted with EtOAc (3¡Á100mL). The combined organic layers were passed through a phase separator and concentrated. The crude material was purified using Teledyne ISCO Combi-Flash system (solid loading, 40G column, 40-80% EtOAc, 20min run) to give 2-(4-chloro-3-methyl-benzoyl)benzoic acid 7 (4.67g, 50.4% yield) as a white solid. 1H NMR (400MHz, CDCl3) delta (ppm): 8.10 (d, J=7.8Hz, 1H), 7.68 (dt, J=7.6, 1.2Hz, 1H), 7.64-7.62 (m, 1H), 7.59 (dt, J=7.9, 1.2Hz, 1H), 7.44 (dd, J=8.2, 2.2Hz, 1H), 7

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; McGowan, Kevin M.; Nance, Kellie D.; Cho, Hykeyung P.; Bridges, Thomas M.; Jeffrey Conn; Jones, Carrie K.; Lindsley, Craig W.; Bioorganic and Medicinal Chemistry Letters; vol. 27; 6; (2017); p. 1356 – 1359;,
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. 62356-27-8, name is 1-Bromo-3-chloro-2-methylbenzene, This compound has unique chemical properties. The synthetic route is as follows., name: 1-Bromo-3-chloro-2-methylbenzene

Embodiment 48 (S,E)-2-(2,6-Dimethoxy-4-(2-(4′-methoxy-2-methylbiphenyl-3-yl)vinyl)benz ylamino)-3 -hydroxypropionic acid 48 Synthetic route Synthesis of compound 48-c 2-Bromo-6-chlorotoluene (8.0g, 38.93mmol) and vinylboronic acid pinacol ester (7.3g, 46.72mmol) were dissolved in toluene (100mL), followed by addition of bis(tri-tert-butylphosphine)palladium (1.4g, 2.73mmol) and triethylamine (35.52g, 311.44mmol). After the reaction system was purged three times with nitrogen, the reaction solution was heated to 80C and stirred for 16 hours. Then the reaction solution was cooled to room temperature, diluted with ethyl acetate (100mL), washed successively with water (100mL x 3) and saturated brine (100mL). The organic phase was dried over anhydrous sodium sulfate. The residue was purified by silica gel column chromatography (petroleum ether) to give compound 48-c (7.19g, yield 65.8%). 1H NMR (400 MHz, CDCl3) delta: 7.66-7.61 (d, J = 23.0Hz, 1H), 7.42-7.41 (d, J = 9.5Hz, 1H), 7.32-7.30 (d, J = 9.5Hz, 1H), 7.13-7.09 (t, 1H), 6.06-6.02 (d, J = 22.5Hz, 1H), 2.45 (s, 3H), 1.32 (s, 12H) ppm.

According to the analysis of related databases, 62356-27-8, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Guangzhou Maxinovel Pharmaceuticals Co., Ltd.; WANG, Yuguang; XU, Zusheng; WU, Tianzhi; HE, Min; ZHANG, Nong; (113 pag.)EP3483142; (2019); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 93-50-5, These common heterocyclic compound, 93-50-5, name is 4-Chloro-2-methoxyaniline, 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.

To a solution of 8-chloro-4-oxo-chromene-2-carboxylic acid (Int-1, lg, 4.45 mmol) in DCM (20 mL) was added 4-chloro-2-methoxyaniline (842 mg, 5.34 mmol), DIPEA (1.15 g, 8.9 mmol) and HATU (3.3 g, 8.9 mmol) at room temperature and the resulting mixture was then stirred at room temperature for 18 hours. After the reaction was completed, the mixture was diluted with water (30 mL) and extracted with EtOAc (50 mL) three times. The combined organic layer was washed with brine, dried over anhydrous Na2S04 and concentrated in vacuo. The residue was purified by silica gel flash chromatography (elution with PE/EtOAc=lO:l~l:3) to give 8-chloro-N-(4-chloro-2-methoxyphenyl)-4-oxo-chromene-2-carboxamide (1.3 g, 80.3 %) as a yellow solid. MS obsd. (ESI+) [(M+H)+]: 364.1.

The synthetic route of 93-50-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; F. HOFFMANN-LA ROCHE AG; HOFFMANN-LA ROCHE INC.; FENG, Song; LIANG, Chungen; LIU, Yongfu; TAN, Xuefei; WU, Jun; WANG, Jianping; (134 pag.)WO2020/79106; (2020); 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. 932-32-1, name is 2-Chloro-N-methylaniline belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. name: 2-Chloro-N-methylaniline

Weigh BTC (58mg, 0.2mmol) in a 25mL two-neck bottle.Add 5 mL of anhydrous dichloromethane, magnetically stir, add equivalents of N-methyl-o-chloroaniline, triethylamine (0.25 mmol) and 5 mL of dichloromethane in a 25 mL constant pressure dropping funnel.Under the ice bath,Slowly add dropwise, remove the ice salt bath after the end of the addition, and stir at room temperature for 4 h.HZA (40 mg, 0.1 mmol) was added to a 10 ml vial, and traces of DMAP, 5 mL of dichloromethane were added, and magnetically stirred at room temperature until completely dissolved. The solution was slowly added dropwise to the above reaction solution under ice salt bath, and the ice salt bath was removed by dropwise addition, and stirred at room temperature. After the reaction is completed, 3 to 6 times the volume of the reaction liquid is added to the above reaction liquid, and distilled water is added.The organic layer was extracted with EtOAc (EtOAc) (EtOAc m.The crude product was then eluted with a petroleum ether:ethyl acetate volume ratio of 20:1 in a mixed solvent, and a thin layer was detected to collect an eluent having a strong ultraviolet at 254 nm and a polarity less than HZA.The combined eluate and the product obtained by evaporating the solvent under reduced pressure are dried to obtain HZAM-12.The yield was 88%.

The synthetic route of 932-32-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Zhejiang University of Technology; Zhan Zhajun; Shan Weiguang; Chen Yan; Shu Renhuan; Wang Jianwei; Ma Liefeng; (31 pag.)CN109956952; (2019); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics