反应详情

To a stirred refluxing mixture of 3-cyano-4-nitrobenzophenone (Method 6) (1.50 g) and iron powder (3.64 g) in ethanol (50 ml) was added dropwise over 0.5 hour a solution of concentrated hydrochloric acid (0.35 ml) in ethanol (14 ml) and reflux was maintained overnight. The hot mixture was filtered through diatomaceous earth and the reaction flask and diatomaceous earth pad was washed with three 50 ml portions of ethanol. The combined filtrate was evaporated to yield a tan solid. Chromatography (eluent 10% to 40% ethyl acetate gradient in dichloromethane) gave the title compound (0.21 g) as a tan solid. M.p. 158-160° C.;

1. temperatureTo a stirred refluxing
2. temperaturereflux
3. temperaturewas maintained overnight
4. filtrationThe hot mixture was filtered through diatomaceous earth
5. washthe reaction flask and diatomaceous earth pad was washed with three 50 ml portions of ethanol
6. customThe combined filtrate was evaporated
7. customto yield a tan solid