反应详情

温度

20 °C

To 16.8 g (73 mmole) of 2-dimethylamino-4'-difluoromethoxyacetophenone in 100 ml of methylene chloride cooled to 0° C. was added 7.6 g (81 mmole) of methyl chloroformate. After the addition was complete the reaction mixture was allowed to warm to 20° C. and stirred overnight. Concentration in vacuo, partitioning between diethyl ether and 1M aqueous hydrochloric acid, washing with brine, drying over anhydrous magnesium sulfate, and reconcentration in vacuo gave a crude oil. Chromatography of this oil on silica gel using diethyl ether in hexanes gave 12 g of 2-(N-methyl-N-(methoxycarbonyl)amino)-4'-difluoromethoxyacetophenone an oil, bp 150°-190° C. at 0.7 torr.

1. additionAfter the addition
2. concentrationConcentration in vacuo
3. custompartitioning between diethyl ether and 1M aqueous hydrochloric acid
4. washwashing with brine
5. dry with materialdrying over anhydrous magnesium sulfate, and reconcentration in vacuo
6. customgave a crude oil