反应详情

温度

90 °C

A mixture of methyl 2-[2-(6-chloropyrimidin-4-yloxy)phenyl]-3,3-dimethoxypropanoate (17.98 g), acetic anhydride (5.16 g) and toluene (73 ml) was stirred at 90° C. for 20 minutes. Methane sulphonic acid (0.49 g) was added to the mixture and the mixture was heated at 90° C. for 1 hour. The mixture was cooled to room temperature, washed with cold water (25 ml) and with hot (50° C.) water (2×25 ml). The organic layer was evaporated at 75° C. (initially on a rotary evaporator, then at circa 15 mm Hg) to leave (E)-methyl 2-[-(6-chloropyrimidin-4-yloxy)phenyl]-3-methoxypropenoate as a solid (16.1 g).

1. temperaturethe mixture was heated at 90° C. for 1 hour
2. temperatureThe mixture was cooled to room temperature
3. washwashed with cold water (25 ml) and with hot (50° C.) water (2×25 ml)
4. customThe organic layer was evaporated at 75° C. (
5. custominitially on a rotary evaporator