Synthetic Route of 630-22-8,Some common heterocyclic compound, 630-22-8, name is 2,2-Dimethylpropanethioamide, molecular formula is C5H11NS, 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 2-propen-1 -yl {3-[(2-chloro-4-pyrimidinyl)acetyl]-2- fluorophenyl}carbamate (30 g, 85.9 mmol) in DMA (300 ml_), NBS (15.3 g, 85.9 mmol) was added. The reaction mixture was stirred at room temperature for 1 h. Then 2,2-dimethylpropanethioamide (1 1 .0 g, 94.5 mmol) was added at 0 C. The mixture was stirred at room temperature for 2 h. The mixture was poured into water and extracted with EtOAc (200 ml_ x 3). The combined organic layers were washed with water and brine successively, dried over Na2SO , filtered and concentrated under reduced pressure to give the crude product, which was purified by column chromatography on silica gel(DCM etroleum ether 2:1 ) to afford the title compound. 1 1 g (35.4 % yield) 1 H NMR (400 MHz, CDCI3) delta ppm 8.29 (d, J=5.27 Hz, 1 H), 8.12-8.19 (m, 1 H), 7.12-7.25 (m, 2H), 6.80-6.88 (m, 2H), 5.85-5.98 (m, 1 H), 5.20-5.37 (m, 2H), 4.61 -4.67 (m, 2H). MS (ES+): 447 [M+H]+ .
The synthetic route of 630-22-8 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; GLAXOSMITHKLINE LLC; ADAMS, Jerry, Leroy; FAITG, Thomas; KASPAREC, Jiri; PENG, Xin; RALPH, Jeffrey; RHEAULT, Tara Renae; WATERSON, Alex Gregory; WO2011/59610; (2011); A1;,
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