反应详情

A cooled (0° C.) solution of 6-chloro-N-(2-methylphenyl)pyrimidine-4-carboxamide (Intermediate 18; 14.00 g; 56.52 mmol) in DCM (280 ml) was treated dropwise with a solution of chlorosulfonic acid (37.8 ml; 565 mmol) in DCM (100 mL). The reaction mixture was allowed to warm from 0° C. to room temperature, then it was stirred at room temperature overnight. The mixture was cooled to 15° C., a mixture ice/water was added and it was stirred for a few minutes. Phases were separated and the organic layer was washed with cold water, brine, dried over MgSO4, filtered and concentrated under vacuum to afford the title compound as a beige solid.

1. temperatureto warm from 0° C. to room temperature
2. temperatureThe mixture was cooled to 15° C.
3. stirringit was stirred for a few minutes
4. customPhases were separated
5. washthe organic layer was washed with cold water, brine
6. dry with materialdried over MgSO4
7. filtrationfiltered
8. concentrationconcentrated under vacuum