反应详情

温度

120 °C

Under a stream of argon, to compound (3) (5.2 g; 24.2 mmol), dimethyl sulfate (22.1 g; 175 mmol) was added at room temperature over 10 minutes. The reaction temperature was raised to 120° C. and the resulting reaction mixture was stirred for 1 hour and then cooled to room temperature. Diethyl ether was added thereto and light brown crude crystals which precipitated out were separated by filtration. The obtained crude crystals were washed with a solution of diethyl ether/ethanol=1/1 to 1/2 and dried under reduced pressure to give 6.17 g of the title compound (4).

1. customthe resulting reaction mixture
2. temperaturecooled to room temperature
3. customlight brown crude crystals which precipitated out
4. customwere separated by filtration
5. customThe obtained crude crystals
6. washwere washed with a solution of diethyl ether/ethanol=1/1 to 1/2
7. customdried under reduced pressure