Category: 630-22-8

Related Products of 630-22-8, 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. 630-22-8 name is 2,2-Dimethylpropanethioamide, 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 solution of ethyl 3-bromopyruvate (1.95 g, 10 mmol, 1.0 eq) and 2, 2, 2-trimethyl-thioacetamide (1.17 g, 10 mmol, 1.0 eq) in 20 mL of ethanol was stirred at room temperature for 48 h. The solvent was evaporated under reduced pressure, and the residue was extracted with aqueous sodium bicarbonate and DCM. The DCM layer was dried over anhydrous magnesium sulfate and evaporated to dryness. The residue was separated by column chromatography to give 2-tert-butyl-thiazole-5-carboxylic acid ethyl ester as a colorless oil (1.15 g, 55.0% yield). 1H NMR (400 MHz, CDCl3) delta 8.01 (s, 1H), 4.38 (q, J=7.1 Hz, 2H), 1.46 (s, 9H), 1.37 (t, J=7.1 Hz, 3H). MS m/z (ESI): 214.0 [M+H].

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

Reference:
Patent; Si Chuan University; Yang, Shengyong; Wei, Yuquan; (168 pag.)US2017/305920; (2017); A1;,
Amide – Wikipedia,
Amide – 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. 630-22-8, name is 2,2-Dimethylpropanethioamide, A new synthetic method of this compound is introduced below., 630-22-8

To a solution of N-(3-(2-bromo-2-(2-(methylthio)pyrimidin-4-yl)acetyl)-2- chloro-5-fluorophenyl)-pivalamide (AT, 489 mg, 1.03 mmol) in DMA (4.7 mL) under Ar at rt was added 2,2-dimethylpropanethioamide (131 mg, 1.12 mmol). The reaction mixture was stirred at rt for 1 h, and then heated to and maintained at 80 C for 3 h. The reaction was judged complete by LCMS. The reaction mixture was diluted with water and twice extracted with EtOAc. The organic phases were combined, washed with brine, dried (Na2S04), and concentrated. The resulting residue was adsorbed onto silica gel and purified by flash chromatography on silica gel using an EtOAc :heptanes (0-15%) elution gradient to furnish N-(3 -(2 -tert-butyl-5 -(2-(methylthio)pyrimidin-4-yl)thiazol-4-yl)-2-chloro-5 – fluorophenyl)pivalamide (175 mg, 0.36 mmol, 38 %) as a white foam: LCMS (m/z): 493.1 (MH+), tR = 1.42 min.

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; NOVARTIS AG; MADERA, Ann Marie; POON, Daniel; SMITH, Aaron; WO2011/161216; (2011); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

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. 630-22-8 name is 2,2-Dimethylpropanethioamide, 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. 630-22-8

N-Bromosuccinimide (107mg, 0.60mmol) was added to a solution of tert-bv yl (3-(2-(2- chloropyrimidin-4-yl)acetyl)-2-fluorophenyl)carbamate (200. Omg, 0.54mmol) in dimethylacetamide (5.5mL). The reaction mixture was stirred at room temperature for lh then 2,2,2-Trimethylthioacetamide (70mg, 0.60mmol) was added. After stirring at room temperature for lh, the medium was heated at 50C overnight. The mixture was poured onto water and the suspension was filtered. The solid was dried under vacuum to afford the title (220mg, 86%). LC/MS (ES+): 463.3-465.3 (M+l).

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

Reference:
Patent; CELLIPSE; PRUDENT, Renaud; PAUBLANT, Fabrice; (74 pag.)WO2018/55097; (2018); A1;,
Amide – Wikipedia,
Amide – 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. 630-22-8, name is 2,2-Dimethylpropanethioamide, A new synthetic method of this compound is introduced below., 630-22-8

at room temperature, to dimethylacetamide (35mL) in a (3- (2- (t-butyl) -5- (2-chloro-pyrimidin-4-yl) thiazol-4-yl) -2-fluorophenyl ) allyl carbamate (3.21g, 9.18mmol, 1.0eq.) was added N- succinimide (1.64g, 9.21mmol, 1.0eq.).When LCMS showed complete disappearance of the starting material, 2,2,2-trimethoxy thio acetamide (1.3g, 11.1mmol, 1.2eq.) And the reaction was heated overnight at 60 deg.] C.LCMS showed the reaction was complete.The reaction was poured into water (250mL), and extracted with ethyl acetate content.Extract was dried over sodium sulfate, filtered, and concentrated under reduced pressure.With 20% ethyl acetate / heptane, silica gel chromatography (300g, 3 “diameter column) to give the crude product, in the form of an oil to provide (3- (2- (t-butyl) -5- (2- chloro-pyrimidin-4-yl) thiazol-4-yl) – 2-fluorophenyl) allyl carbamate (2.92g, 70% yield)

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; Pulaixike Company; Zhang, Chao; Ibrahim, Prabha N; Nespi, Marika; Shi, Songyuan; Spevak, Wayne; Habets, Gaston G; Burton, Elizabeth A; Hirth, Klaus-Peter; (181 pag.)CN105228983; (2016); A;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

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. 630-22-8 name is 2,2-Dimethylpropanethioamide, 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. 630-22-8

General procedure: To a suspension of different thioamides 1b, 2b, 3b (7.28 mmol)in ethyl alcohol (15 mL) was added at room temperature ethyl 2-chloroacetoacetate (1 equiv.). The solution was refluxed for 24 h,and then the solvent was removed under reduced pressure. Thesolid material was washed with cooled hexane (2 10 mL) to givethe corresponding pure ethyl carboxylate derivatives 1c, 2c, 3c indifferent yields. Ethyl 2-(tert-butyl)-4-methylthiazole-5-carboxylate (1c).Prepared from 2,2-dimethyl propanthioamide (1b). Yellow solid75.3%; mp: 43e47 C [40].

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

Reference:
Article; Ghonim, Aya E.; Ligresti, Alessia; Rabbito, Alessandro; Mahmoud, Ali Mokhtar; Di Marzo, Vincenzo; Osman, Noha A.; Abadi, Ashraf H.; European Journal of Medicinal Chemistry; vol. 180; (2019); p. 154 – 170;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

A common heterocyclic compound, 630-22-8, name is 2,2-Dimethylpropanethioamide, molecular formula is C5H11NS, 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. 630-22-8.

Intermediate 23: 2-Propen-1-yl {3-[5-(2-chloro-4-pyrimidinyl)-2-(1,1-dimethylethyl)-1,3-thiazol-4-yl]-2-fluorophenyl}carbamate; To a solution of 2-propen-1-yl {3-[(2-chloro-4-pyrimidinyl)acetyl]-2-fluorophenyl}carbamate (30 g, 85.9 mmol) (Intermediate 20) in DMA (300 mL), NBS (15.3 g, 85.9 mmol) was added. The reaction mixture was stirred at rt for 1 h. Then 2,2-dimethylpropanethioamide (11.0 g, 94.5 mmol) was added at 0 C. The mixture was stirred at rt for 2 h. The mixture was poured into water and extracted with EtOAc (200 mL¡Á3). The combined organic layers were washed with water and brine successively, dried over Na2SO4, filtered and concentrated under reduced pressure to give the crude product, which was purified by column chromatography on silica gel (DCM:petroleum ether 2:1) to afford the title compound. (11 g, 35.4% yield). 1H NMR (400 MHz, CDCl3) delta ppm 8.29 (d, J=5.27 Hz, 1H), 8.12-8.19 (m, 1H), 7.12-7.25 (m, 2H), 6.80-6.88 (m, 2H), 5.85-5.98 (m, 1H), 5.20-5.37 (m, 2H), 4.61-4.67 (m, 2H). MS (ES+): 447 [M+H]+.

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

Reference:
Patent; Adams, Jerry Leroy; Dickerson, Scott Howard; Johnson, Neil W.; Kuntz, Kevin; Petrov, Kimberly; Ralph, Jeffrey M.; Rheault, Tara Renae; Schaaf, Gregory; Stellwagen, John; Tian, Xinrong; Uehling, David Edward; Waterson, Alex Gregory; Wilson, Brian; US2009/298815; (2009); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics