反应详情

温度

0 °C

To a solution of 3-ethoxy-N-methoxy-N-methyl-4-trifluoromethyl-benzamide from step 7 (15.96 g, 58 mmol) in THF (182 mL) at −5° C. was added methylmagnesium bromide (3 M in Et2O, 38.37 mL, 115 mmol). The mixture was stirred at 0° C. for 15 min, then warmed up to 23° C., stirring was continued for further 3 h at 23° C. Cooled to 0° C., 1 N HCl (274 mL) was added dropwise, stirring was continued at 23° C. for 15 min, the mixture was diluted with TBME, the phases were separated, the organic layer was washed with water and brine, dried over MgSO4. Removal of the solvent in vacuum left a yellow solid (13.10 g, 98%), which was used without further purification. MS (EI) 232.2 [M].

1. temperaturewarmed up to 23° C.
2. stirringstirring
3. waitwas continued for further 3 h at 23° C
4. temperatureCooled to 0° C.
5. stirringstirring
6. waitwas continued at 23° C. for 15 min
7. customthe phases were separated
8. washthe organic layer was washed with water and brine
9. dry with materialdried over MgSO4
10. customRemoval of the solvent in vacuum
11. waitleft a yellow solid (13.10 g, 98%), which
12. customwas used without further purification