反应详情

Crude allyl 3-nitrocinnamate (3 g, 12.9 mM) was dissolved in ethyl acetate (10 ml) and added slowly to a stirred suspension of SnCl2.2H2O(14.52 g, 64 mM) in ethyl acetate (20 ml). The mixture was refluxed under argon for 3 hours, cooled, and poured into a mixture of ammonia (sg 880, 15 ml) and water (5 ml). Ethyl acetate (50 ml) was added, and the organic layer separated by decantation. Two further extractions with ethyl acetate (each 50 ml) were made similarly. The combined extracts were washed with water and brine, dried (MgSO4) and evaporated to give title compound (2.6 g).

1. temperatureThe mixture was refluxed under argon for 3 hours
2. temperaturecooled
3. customthe organic layer separated by decantation
4. extractionTwo further extractions with ethyl acetate (each 50 ml)
5. washThe combined extracts were washed with water and brine
6. dry with materialdried (MgSO4)
7. customevaporated