反应 #2129607
相关文献 (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US08697737B2
反应条件: temp:100.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: To acetic anhydride (20 mL) was added 2-chloro-4,5-difluoroaniline (4.7 g, 29 mmol), and the resulting solution was stirred at 100° C. for 1 h. After cooling to rt, the mixture was stored in a freezer overnight. A white crystalline precipitate formed, and it was collected by filtration. Residual acetic anhydride was removed in vacuo. The desired N-(2-chloro-4,5-difluorophenyl)acetamide (4.69 g, 22.8 mmol, 79% yield) was isolated as a white crystalline solid. 1H NMR (400 MHz, CDCl3): 8.38 (dd, 1H), 7.53 (br s, 1H), 7.23 (dd, 1H), 2.25 (s, 3H); MS (EI) for C8H6ClF2NO: 206 (MH+). After cooling to rt the mixture was stored in a freezer overnight A white crystalline precipitate formed it was collected by filtration Residual acetic anhydride was removed in vacuo
来源 ID: ord-687fc455ffd5437597270ee905d399a3