Tag: M.W=200-300

Related Products of 63624-28-2,Some common heterocyclic compound, 63624-28-2, name is 2,4-Dimethoxybenzene-1-sulfonyl chloride, molecular formula is C8H9ClO4S, 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.

301 mg of the compound obtained in step 16-2 (diastereoisomer mixture) was added under ice cooling and a nitrogen atmosphere to a 3 mL tetrahydrofuran solution of 26 mg of sodium hydride, and the reaction mixture was stirred for 20 minutes. After this, a 2 mL tetrahydrofuran solution of 170 mg of 2,4-dimethoxybenzenesulfonyl chloride was added dropwise, and the reaction mixture was stirred for 2 hours at room temperature. Then 5mL of ethylacetate and 10mL of a 5% potassium carbonate aqueous solution were added and the reaction mixture was stirred for 30 minutes at room temperature. After liquid separation, the aqueous layer was extracted with ethyl acetate (10 mL × 3), and the combined organic layer was dried with sodium sulfate, after which the drying agent was filtered off and the solvent was distilled off under reduced pressure. The residue thus obtained was separated and purified by column chromatography (silica gel 60, mobile phase: ethyl acetate/acetone = 99/1; v/v) to obtain two kinds of diastereoisomer of the titled compound in amounts of 115 mg (isomer A: colorless, amorphous) and 127 mg (isomer B: colorless, amorphous). Isomer A: [alpha]D25 = -248 (c = 0.183, chloroform) MS (ESI pos.) m/z : 680([M+H]+), (ESI pos.) m/z : 702([M+Na]+ 1H-NMR (499 MHz, CDCl3) delta (ppm) ; 1.89 (s, 1 H), 2.19 – 3.94 (m, 21 H), 4.65 – 5.06 (m, 1 H), 5.23 – 5.44 (m, 1 H), 6.43 (s, 1 H), 6.57 (dd, J =9.0, 2.3 Hz, 2 H), 6.97 – 7.05 (m, 1 H), 7.42 (d, J=8.8 Hz, 1 H), 7.75 (s, 1 H), 7.93 (d, J=8.5 Hz, 1 H), 8.09 – 8.20 (m, 1 H) Isomer B: [alpha]D25 = +211 (c = 0.200, chloroform) MS (ESI pos.) m/z : 680([M+H]+), (ESI pos.) m/z : 702([M+Na]+) 1 H-NMR (499 MHz, CDCl3) delta (ppm) ; 1.88 – 2.23 (m, 2 H), 2.33 (s, 3 H), 2.55 – 2.81 (m, 6 H), 3.36 (s, 3 H), 3.47 – 3.63 (m, 1 H), 3.79 – 3.88 (m, 7 H), 4.07 – 4.19 (m, 1 H), 4.95 – 5.19 (m, 1 H), 6.48 (d, J=2.1 Hz, 1 H), 6.57 (dd, J=8.8, 2.1 Hz, 1 H), 6.63 (d, J=8.2 Hz, 1 H), 6.99 – 7.07 (m, 1 H), 7.41 – 7.48 (m, 1 H), 7.67 (s, 1 H), 7.92 – 8.01 (m, 1 H), 8.13 (d, J=8.8 Hz, 1 H)

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2,4-Dimethoxybenzene-1-sulfonyl chloride, its application will become more common.

Reference:
Patent; TAISHO PHARMACEUTICAL CO., LTD; EP1659121; (2006); A1;,
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Electric Literature of 39226-96-5, 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. 39226-96-5, name is (2-Chloro-3-(trifluoromethyl)phenyl)methanamine belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

3) N-(2-chloro-3-(trifluoromethyl)benzyl)-3-cyclopropyl-1-methyl-1H-pyrazole-5-carboxamide To a solution of amine (500 mg, 2.39 mmol, 1.0 eq) and acid (397 mg, 2.39 mmol, 1.0 eq) in DMF (15 mL) were added DIEA (1.54 g, 11.9 mmol, 5 eq) and HBTU (1.09 mg, 12.87 mmol, 1.2 eq) and the reaction mixture was stirred at rt for 12 h. The reaction mixture was then diluted with ethyl acetate (20 mL) and washed with 10% aqHCl (1*20 mL), sat NaHCO3 (1*20 mL) and water (4*20 mL). Organic layer was collected, dried (MgSO4) and evaporated to give a crude product, which was purified by column chromatography (EtOAc/Hexane 10% to 50%) to give the desired product. Mass Spectrum (LCMS, ESI Pos.) Calcd. For C16H16ClF3N3O: 358.0 (M+H), Found 358.0.

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, (2-Chloro-3-(trifluoromethyl)phenyl)methanamine, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Prosetta Antiviral ,Inc.; Selvarajah, Suganya; Paulvannan, Kumar; (58 pag.)US2018/118679; (2018); A1;,
Chloride – Wikipedia,
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Related Products of 41965-95-1, 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. 41965-95-1 name is 3-Chloro-4-methoxybenzylamine Hydrochloride, 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.

General procedure N: Amide coupling (10):In a glass vial, under inert atmosphere (N2), to a solution of the carboxylic acid (1.0 eq.) in CH2CI2 (0.25 M) were added HOBt (1.20 eq.), DMAP (0.25 eq.), EDC HCI (2.5 eq.) and DIPEA (4.0 eq.). The reaction mixture was stirred at rt for 30 min. An amine (2.0 eq.) was then added and the reaction mixture stirred at rt until completion of the reaction. DMF (0.3 vol. CH2CI2) and PL-SO2CI2 (1.0 eq.) were added and after stirring at rt for 1 h the mixture was filtered (CH2CI2) and concentrated under reduced pressure. Purification of the residue by FC or HPLC gave the desired compound.; Example 374:(Sf^-Lambda/^S-Chloro^-methoxyphenyl-methyO-tef^-Lambda^^-pyrrolidino-butyO^S*^/?*)- [4,7-ethenylene-spiro[2.4]heptane]-5,6-dicarboxamide, formate salt:Following general procedure N, starting from (5R*)-5-hydroxycarbonyl-(6R*)-Lambda/6-(4- pyrrolidin-1-yl-butyl)-(4S*,7/?*)-[4,7-ethenylene-spiro[2.4]heptane]-6-carboxamide and 3- chloro-4-methoxybenzylamine hydrochloride.LC-MS-conditions FA: tR = 0.75 min; [M+H]+ = 486.24.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 3-Chloro-4-methoxybenzylamine Hydrochloride, and friends who are interested can also refer to it.

Reference:
Patent; ACTELION PHARMACEUTICALS LTD; BUR, Daniel; CORMINBOEUF, Olivier; CREN, Sylvaine; GRISOSTOMI, Corinna; LEROY, Xavier; RICHARD-BILDSTEIN, Sylvia; WO2010/134014; (2010); A1;,
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Application of 13918-92-8, The chemical industry reduces the impact on the environment during synthesis 13918-92-8, name is 2,4-Difluorobenzene-1-sulfonyl chloride, I believe this compound will play a more active role in future production and life.

General procedure: Compound 11a (800 mg,2.0 mmol) was dissolved in 10 ml ethyl acetate and then 9 N HCl(5 ml) was added, the reaction mixture was stirred for 30 min at roomtemperature, the reaction solvent was neutralized by NaHCO3 topH=8, 50 ml ethyl acetate and 30 ml H2O was added, after stirredadequately, the organic layer was separated, and concentrated, andthen the crude product was purified by silica gel columnchromatography using a mixture solvent of dichloromethane:methanol (20:1), to give white powder (540 mg); Above whitepowder (150 mg, 0.5 mmol) was dissolved in THF (10 ml),iodomethane (107 mg, 0.75 mmol) and triethylamine (0.5 ml) wereadded in the solvent. After the reaction mixture was stirred for 1 h at room temperature, the solvent was concentrated, the residues was purified by silica gel column chromatography using a mixture solvent ofdichloromethane: methanol (40:1), to give (12aa) Yield 49%, White powder.

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; Zhang, Min; Jiang, Li; Tao, Jia; Pan, Zhaoping; He, Mingyao; Su, Dongyuan; He, Gu; Jiang, Qinglin; Bioorganic and Medicinal Chemistry; vol. 27; 11; (2019); p. 2268 – 2279;,
Chloride – Wikipedia,
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Reference of 328-84-7, 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. 328-84-7, name is 3,4-Dichlorobenzotrifluoride belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

a. 1,3-Bis(2-chloro-alpha,alpha,alpha-trifluoro-p-tolyloxy)benzene A solution of potassium hydroxide (3.26 g. 0.05 mole, 85%) in water (~3 g.) is added slowly dropwise to a solution of resorcinol (2.75 g. 0.025 mole) and 3,4-dichloro-alpha,alpha,alpha-trifluorotoluene (10.75 g. 0.05 mole) in sulfolane (125 ml) at 150-160 C., with stirring. When the addition is complete, the strongly colored reaction mixture is stirred at 150-160 C. overnight, then cooled, diluted with benzene (200 ml), and washed cautiously with water (700 ml). Hexane (200 ml) is added and the mixture washed with water (600 ml), dilute sulfuric acid (600 ml), dilute sodium hydroxide solution (600 ml), and water (600 ml), dried, and the solvent removed to give 1,3-bis(2-chloro-alpha,alpha,alpha-trifluoro-p-tolyloxy)benzene (8.6 g. 65%) b.p. 160-70 C./0.1 mm.

The synthetic route of 3,4-Dichlorobenzotrifluoride has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Rohm and Haas Company; US31455; (1983); E1;; ; Patent; Rohm and Haas Company; US4063929; (1977); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Related Products of 38762-41-3, A common heterocyclic compound, 38762-41-3, name is 4-Bromo-2-chloroaniline, molecular formula is C6H5BrClN, 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: Experimental Procedure: A dried 25 mL Schlenk tube equipped with a magnetic stir bar was charged with Togni?s Reagent 2 (0.25 mmol, 1.0 equiv), free anilines 1 (0.75 mmol, 3.0 equiv), K2CO3 (0.375 mmol, 1.5 equiv) and CH3CN (1.5 mL). The reaction mixture was then stirred at 75 C for 6 h under an argon atmosphere. The reaction progress was monitored by TLC. After cooling to room temperature, the mixture was washed with water and extracted with CH2Cl2 three times, then washed with saturated NaCl solution. The combined organic layer was dried with anhydrous Na2SO4 and filtered. The filtrate was concentrated in vacuo. The crude product was purified by flash column chromatography on silica gel (Elutent: petroleum ether-EtOAc) to give the pure product. The products were characterized by 1H NMR, 13C NMR, 19F NMR, GC -MS.

The synthetic route of 38762-41-3 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Chen, Xiaoyu; Ding, Licheng; Li, Linlin; Li, Jingya; Zou, Dapeng; Wu, Yangjie; Wu, Yusheng; Tetrahedron Letters; vol. 61; 9; (2020);,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 38762-41-3, name is 4-Bromo-2-chloroaniline, 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 38762-41-3, COA of Formula: C6H5BrClN

General procedure: A dried tube, equipped with a magnetic stirred and a septum, 2-chloroanilines (1.0 mmol) was dissolved in DMSO(3 mL), and t-BuOK (3 mmol) was added. The mixture was stirred for 5 minutes, and thendimethylthiocarbamoyl chloride (1.2 mmol) and bis(dibenzylideneacetone) palladium (5 mol%) were added.the reaction mixture was then heated at 100 C and checked by TLC until the starting material was finished. Thereaction was cooled down to room temperature, and then quenched with sat. NH4Cl solution (5 mL) and extractedwith ethyl acetate, dried over anhydrous Na2SO4 and evaporated under vacuum. The residue was purified by flashcolumn chromatography to afford the desired product.

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, 4-Bromo-2-chloroaniline, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Xu, Wan; Zeng, Meng-Tian; Liu, Min; Liu, Xing; Chang, Cai-Zhu; Zhu, Hui; Li, Yue-Sheng; Dong, Zhi-Bing; Chemistry Letters; vol. 46; 5; (2017); p. 641 – 643;,
Chloride – Wikipedia,
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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. SDS of cas: 202197-26-0

General procedure: To a solution of 4-chloro-7-fluoro-6-nitroquinazoline (4.58 g,20 mmol) in acetonitrile (500 ml) was added 3-chloro-4-(3-fluorobenzyloxy)aniline (4.77 g, 19 mmol), and then the mixturewas raised to reflux. Once the reaction was completed as indicatedby TLC, The precipitate was collected by filtration, and washed withacetonitrile to give N-(3-chloro-4-(3-fluorobenzyloxy)phenyl)-7-fluoro-6-nitroquinazolin-4-amine 7.5 g (16.9 mmol, 85%)

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

Reference:
Article; Zhang, Long; Yang, Yingying; Zhou, Haojie; Zheng, Qingmei; Li, Yuhao; Zheng, Shansong; Zhao, Shuyong; Chen, Dong; Fan, Chuanwen; European Journal of Medicinal Chemistry; vol. 102; (2015); p. 445 – 463;,
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Electric Literature of 53531-69-4, 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. 53531-69-4, name is (4-Bromophenyl)methanesulfonyl chloride belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Diethyl 5-aminobenzofuran-2,3-dicarboxylate (0.8 g, 2.59 mmol), 4-bromobenzylsulfonyl chloride (1.56 g, 5.77 mmol),Potassium carbonate (1.01 g, 7.30 mmol) was successively added to 30 mL of dichloromethane, and the mixture was stirred overnight at room temperature, and potassium carbonate was removed by filtration, and the residue was purified by column chromatography to yield 1.32 g (yield: 89.64%).

The synthetic route of (4-Bromophenyl)methanesulfonyl chloride has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Jiangsu Hengrui Pharmaceutical Co., Ltd.; You Qidong; Wei Jinlian; Jiang Zhengyu; Guo Xiaoke; Xu Xiaoli; Zhang Xiaojin; (44 pag.)CN107619384; (2018); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 771583-81-4, 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. 771583-81-4, name is 4-Chloro-2-(trifluoromethyl)benzylamine, This compound has unique chemical properties. The synthetic route is as follows.

5-((4- (ethylsulfonyl) benzyl) carbamoyl) -2-methoxybenzoic acid (150.0 mg, 0.4 mmol), HATU (302.2 mg, 0.8 mmol) and DIPEA (154.1 mg, 1.2 mmol) was dissolved in tetrahydrofuran (10 mL), and after stirring at room temperature for 0.5 hours, 4-chloro-2- (trifluoromethyl) benzylamine (125.0 mg, 0.6 mmol) was added, and the reaction was performed at room temperature for 4 hours. An appropriate amount of water was added and extracted three times with ethyl acetate. The organic phases were combined and washed with a saturated sodium chloride solution, dried over anhydrous sodium sulfate, filtered, and the filtrate was concentrated. The concentrate was purified by preparative high performance liquid chromatography to obtain the title compound (90.0 mg, yield: 38%).

The chemical industry reduces the impact on the environment during synthesis 4-Chloro-2-(trifluoromethyl)benzylamine. I believe this compound will play a more active role in future production and life.

Reference:
Patent; Sichuan Kelun Botai Bio-pharmaceutical Co., Ltd.; Liu Chunchi; Liu Jinming; Ren Yun; Cai Jiaqiang; Wang Lichun; Wang Jingyi; (42 pag.)CN110724075; (2020); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics