反应详情

温度

15 °C

5 g (0.021 mol) product from example 7b was dissolved in 10 ml 98% methane-sulfonic acid during 10 minutes at 35° C. and was then cooled to 15° C. 5.14 (0.128 mol) 85% hydrogen peroxide was added by drops, the temperature not exceeding 25° C. After 2 hours at 30° C., 400 ml ice-cold (0°-10° C.) ethyl acetate and 100 ml saturated (NH4)2SO4 solution were added and the mixture was allowed to stand for another 2 hours under agitation. The ethyl acetate phase was separated and dried over Na2SO4, whereupon the ethyl acetate was evaporated at 30° C. until a slightly yellow, viscous oil formed. Titration on active oxygen showed a yield of 72%.

1. customexceeding 25° C
2. waitto stand for another 2 hours under agitation
3. customThe ethyl acetate phase was separated
4. dry with materialdried over Na2SO4, whereupon the ethyl acetate
5. customwas evaporated at 30° C. until a slightly yellow, viscous oil
6. customformed