反应详情

温度

120 °C

Under a stream of argon, to compound (7) (24.4 g; 94.2 mmol), dimethyl sulfate (77 g; 610 mmol) was added in an ice bath over 20 minutes. The reaction temperature was raised to 120° C. and the resulting reaction mixture was stirred for 1 hour. To the reaction mixture, diethyl ether was added in an ice bath, and solids which precipitated out were separated by filtration. The resulting solids were washed with a mixed solution of diethyl ether/ethanol (1/1 to 1/2) and dried under reduced pressure to give 33.6 g (yield: 96%) of the title compound (8).

1. customthe resulting reaction mixture
2. customsolids which precipitated out
3. customwere separated by filtration
4. washThe resulting solids were washed with a mixed solution of diethyl ether/ethanol (1/1 to 1/2)
5. customdried under reduced pressure