Category: chlorides-buliding-blocks

Application of 210532-25-5, These common heterocyclic compound, 210532-25-5, name is 3,5-Difluorobenzene-1-sulfonyl chloride, 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.

N-(6-chloro-5-cyanopyridin-3-yl)-3,5-difluorobenzene-sulfonamide 1.132 g (5.32 mmol) of 3,5-difluorobenzene-1-sulfonyle chloride is added under argon to a solution of 545 mg (3.55 mmol) of 5-amino-2-chloronicotinotrile in 20 mL of an anhydrous 1:1 mixture of THF and pyridine. The reaction medium is heated to 70 C. for 3 hours and let 12 additional hours under stirring at room temperature. The solvent is dry evaporated and the crude reaction product is redissolved in ethyl acetate and washed with several aqueous fractions. The organic phase is dried on magnesium sulfate, filtered, concentrated and then purified by silica gel chromatography to yield 784 mg (67%) of N-(6-chloro-5-cyanopyridin-3-yl)-3,5-difluorobenzene-sulfonamide. 1H NMR: deltaH ppm (400 MHz, DMSO): 11.39 (1H, s1, NH), 8. 34 (1H, m, CHarom), 8.10 (1H, m, CHarom), 7.67 (1H, m, CHarom), 7.59 (2H, m, CHarom).

The synthetic route of 210532-25-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; PIERRE FABRE MEDICAMENT; KALOUN, El Bachir; BEDJEGUELAL, Karim; RABOT, Remi; KRUCZYNSKI, Anna; SCHMITT, Philippe; PEREZ, Michel; RAHIER, Nicolas; US2013/85144; (2013); A1;,
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Application of 2106-04-9, A common heterocyclic compound, 2106-04-9, name is 3-Chloro-2-fluoroaniline, molecular formula is C6H5ClFN, 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 2-Fluoro-3-chlorophenylisothiocyanate Into a solution of 2-fluoro-3-chloroaniline (1.0 g, 6.87 mmol) in 30 mL of toluene at room temperature, thiophosgene (0.8 mL, 10.3 mmol) and triethylamine (1.12 mL, 8.24 mmol) were added. The mixture was stirred at room temperature for 16 hours. The mixture was parationed between ethyl acetate and water. The combined organic layer was then concentrated to give the desired product (950 mg, 74%). 1H NMR (CDCl,) delta 7.09 (m, 2H), 7.30 (m, 1H).

The synthetic route of 2106-04-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Palovich, Michael R.; Widdowson, Katherine L.; Nie, Hong; US2003/216375; (2003); A1;,
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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. 104-77-8, name is 3-Chloro-N,N-diethylpropan-1-amine, This compound has unique chemical properties. The synthetic route is as follows., SDS of cas: 104-77-8

a Phenylmethyl 1-[3-(diethylamino)propyl]-1H-indole-3-acetate At a temperature of about +50 C., 6.2 g (44.9 mMol) of potassium carbonate were added to a solution of 4.0 g (15.1 mMol) of phenylmethyl 1H-indole-3-acetate in 40 ml of dimethylformamide and then at the same temperature a solution of 3.0 g (20.0 mMol) of 3-(diethylamino)propylchloride in 5 ml of dimethylformamid were added dropwise. The mixture was stirred for a further hour at 50 C. and overnight at ambient temperature, heated up to 100 C. again and once more 1.0 g of 3-(diethylamino)propylchloride were added. After stirring for 5 hours at ambient temperature, the mixture was stirred into 300 ml of ice water and extracted exhaustively with diisopropylether. The combined organic extracts were washed with saturated saline solution, dried over magnesium sulphate, clarified with activated charcoal and evaporated down under reduced pressure. A colourless oil was obtained in a yield of 5.37 g (94% of theory) and was used in the following step without further purification. MS: M+ =378

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 104-77-8.

Reference:
Patent; Karl Thomae GmbH; US6114390; (2000); A;,
Chloride – Wikipedia,
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Adding a certain compound to certain chemical reactions, such as: 4535-90-4, name is 2-Chloro-N-methylethanamine hydrochloride, 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 4535-90-4, category: chlorides-buliding-blocks

A mixture of iraw5,-8-chloro-l-[4-(3-fluoro-pyridin-2-yl)-cyclohexyl]-5,6-dihydro-4H-2,3,5,10b- tetraaza-benzo[e]azulene (50.0 mg, 0.126 mmol), cesium carbonate (246 mg, 0.754 mmol) and 2-methylaminoethyl chloride hydrochloride (65.4 mg, 0.503 mmol) in acetonitrile (1.3 ml) was heated at 70 C for 20 h. After addition of further portions of cesium carbonate (246 mg, 0.754 mmol) and 2-methylaminoethyl chloride hydrochloride (65.4 mg, 0.503 mmol) the mixture was heated at 70 C for another 20 h. The reaction mixture was partitioned between 1 M aqueous sodium hydroxide solution (2 ml) and ethyl acetate (5 ml). The layers were separated. The aqueous layer was extracted with two 5-ml portions of ethyl acetate. The combined organic layers were concentrated in vacuo. Preparative RP-HPLC with water (0.05% formic acid) / methanol as eluent gave the title compound as formate salt. The salt was partitioned between ethyl acetate (15 ml) and 1 M aqueous sodium hydroxide solution (10 ml). The layers were separated. The aqueous layer was extracted with two 15 ml-portions of ethyl acetate. The combined organic layers were dried over anhydrous sodium sulfate and concentrated in vacuo to give the title compound (14 mg, 25%) as off-white solid. MS m/e: 455 ([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, 2-Chloro-N-methylethanamine hydrochloride, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; F. HOFFMANN-LA ROCHE AG; DOLENTE, Cosimo; SCHNIDER, Patrick; WO2011/131596; (2011); A1;,
Chloride – Wikipedia,
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Reference of 623-12-1,Some common heterocyclic compound, 623-12-1, name is 1-Chloro-4-methoxybenzene, molecular formula is C7H7ClO, 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 appropriate quantity of stock solution C was added to a 4 mL vial containing the aryl chloride (1.00 mmol) and potasium terf-butoxide (123 mg, 1.10 mmol) in 1.5 mL of toluene. The aromatic thiol (1.00 mmol) was then added, and the vial sealed with a cap containing a PTFE septum. The mixture was heated at 110 0C until the chloroarene was consumed, as determined by GC. Silica gel (0.5 g) was then added, and solvents were evaporated under reduced pressure. The crude residue was purified by column chromatography on silica gel using hexane or a mixture of hexane and ethyl acetate as eluent. Aryl sulfides were isolated in the yields reported in Table 4.4-Methoxyphenyl phenyl sulfide (Table 4, entry 1).[49] 100 muL of stock solution C were used. A 50:1 mixture of hexane/ethyl acetate was used as chromatography eluent. 98% yield. Colorless liquid. 1H NMR (CDCl3): delta = 7.23 (d, J= 8.8 Hz5 2H), 7.06-7.02 (m, 2H), 7.00-6.93 (m, 3H), 6.71 (d, J= 8.8 Hz5 2H)5 3.62 (s, 3H). 13C NMR (CDCl3): delta = 159.7, 138.5, 135.3 (2C), 128.8 (2C), 128.1 (2C), 125.7, 124.2, 114.9 (2C)5 55.3.

The synthetic route of 623-12-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; YALE UNIVERSITY; WO2007/64869; (2007); A2;,
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Application of 50594-82-6, These common heterocyclic compound, 50594-82-6, name is 3,4,5-Trichlorobenzotrifluoride, 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.

STR73 12.5 g (0.05 mol) of 3,4,5-trichloro-benzotrifluoride are added slowly and with stirring to a mixture of 8.0 g (0.05 mol) of 2,7-dihydroxynaphthalene, 4.2 g (0.075 mol) of pulverulent potassium hydroxide and 100 ml of dimethyl sulphoxide, which has been warmed to 60 C., and the reaction mixture is then stirred for a further approx. 3 hours at 60 C. After the mixture has been cooled to approximately 20 C., it is diluted with water and methylene chloride, and filtered. The organic phase is separated off from the filtrate, washed with water, dried using sodium sulphate and filtered. The solvent is removed from the filtrate by distillation in a water-pump vacuum, the residue is stirred with petroleum ether and the product which is thus obtained in the form of crystals is isolated by filtering with suction. 4.9 g (26% of theory) of 7-(2,6-dichloro-4-trifluoromethylphenoxy)-2-naphthol of melting point 98 C. are obtained. In analogy to Example (II-1) the starting substances of the formula (II) listed below in Table 2 may be prepared. STR74

The synthetic route of 50594-82-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Bayer Aktiengesellschaft; US5041609; (1991); A;,
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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. 1005-56-7, name is O-Phenyl carbonochloridothioate, A new synthetic method of this compound is introduced below., Safety of O-Phenyl carbonochloridothioate

General procedure: Phenyl chlorothionoformate (345 mg, 2.0 mmol), amine 2 (4.0 mmol) and water (15 mL) were added successively to a 50 mL round-bottom flask. The reaction mixture was stirred at room temperature for 1 h (monitored by TLC). After the reaction was complete, the solid was filtered off, washed with 10% HCl (2 ¡Á 20 mL) and deionised water(2 ¡Á 20 mL), and dried under vacuum to give the pure thiocarbamates 3. All products are known compounds and were identified by comparison of their physical and spectral data with those reported inthe literature.28

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; Li, Zhengyi; Chen, Yuan; Yin, Yue; Wang, Zhiming; Sun, Xiaoqiang; Journal of Chemical Research; vol. 40; 11; (2016); p. 670 – 673;,
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Related Products of 97329-43-6, A common heterocyclic compound, 97329-43-6, name is 1-Bromo-2-chloro-3-methylbenzene, molecular formula is C7H6BrCl, 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 l-(2-chloro-3-methylphenyl)propan-2-one: A Smith process vial was charged with l-bromo-2-chloro-3 -methylbenzene (528 mg, 2.57 mmol, 1 eq.), tributylmethoxytin (1.11 mL, 1.5 eq.), 4-methylpent-4-en-2-one (0.42 mL, 1.5 eq.), PdCl2 (23 mg, 5%) and tri(o-tolyl)phosphine (79 mg, 10%), toluene (1 mL) was added and mixture sparged with nitrogen for 10 minutes and then heated in oil bath at 100 C for 5 hours. The reaction mixture was diluted with ethyl acetate and washed with brine, dried (MgS04), filtered, concentrated and purified by flash column chromatography (silica gel, 0 to 20% ethyl acetate/hexanes) to l -(2-chloro-3-methylphenyl)propan-2- one (375 mg, 80% yield). 1H-NMR: 400 MHz, (CDC13) delta : 7.19-7.02 (m, 3H), 3.82(s, 2H), 2.38(s, 3H), 2.18 (s, 3H).

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; GILEAD SCIENCES, INC.; BABAOGLU, Kerim; BJORNSON, Kyla; GUO, Hongyan; HALCOMB, Randall, L.; LINK, John, O.; MCFADDEN, Ryan; MITCHELL, Michael, L.; ROETHLE, Paul; TRENKLE, James, D.; VIVIAN, Randall, W.; XU, Lianhong; WO2012/3497; (2012); A1;,
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These common heterocyclic compound, 63624-28-2, name is 2,4-Dimethoxybenzene-1-sulfonyl chloride, 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. SDS of cas: 63624-28-2

General procedure: To a mechanically stirred suspension of suspension of 1 (0.21 g, 0.53 mmol) in 30 ml CH2Cl2 were added triethylamine (0.5 ml) and aromatic sulfonyl chloride (0.53 mmol) at 25 C for 4 h. The reaction process was detected by TLC method. Then, antagonized by dilute sodium hydroxide, extracted, and washed with ether and water, evaporated under vacuum. Finally, the mixture was recrys-tallizated from ethyl acetate , providing a total product yield of 65.4%-88.6 %.

The synthetic route of 2,4-Dimethoxybenzene-1-sulfonyl chloride has been constantly updated, and we look forward to future research findings.

Reference:
Article; Wang; Aili; Zhang; Xu; Pharmazie; vol. 74; 2; (2019); p. 73 – 78;,
Chloride – Wikipedia,
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Application of 56961-77-4,Some common heterocyclic compound, 56961-77-4, name is 1-Bromo-2,3-dichlorobenzene, molecular formula is C6H3BrCl2, 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.

29.3 g (100.0 mmol) of Compound 1-A, 22.6 g (100.0 mmol) of Compound 1-B, 2.7 g (3.0 mmol) of Pd2(dba)3, 1.3 g (6.0 mmol) of PtBu3 (50% solution in toluene), 28.8 g (300.0 mmol) of NaOtBu were mixed with 1,500 mL of toluene under a nitrogen (N2) atmosphere, followed by stirring under reflux to allow a reaction to occur for 12 hours. At room temperature, an organic layer was separated therefrom using water and ethyl acetate, and the solvent was dried. Then, through silica gel column chromatography, 28.5 g of compound 49-C was obtained at a yield of 65%. [0352] MS (MALDI-TOF) m/z: 438 [M]+

The synthetic route of 56961-77-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Samsung Display Co., Ltd.; KIM, Myeongsuk; YE, Jimyoung; YOO, Byeongwook; JEONG, Jaeho; (102 pag.)US2020/98991; (2020); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics