反应详情

A suspension of 4-benzyl 1-tert-butyl 2-(4-bromophenyl)succinate (3.00 g, 7.15 mmol) and silica gel (35.7 g) in toluene (230 mL) was heated at reflux for 3 h. The crude mixture was cooled to room temperature and filtered. The filter cake was washed with dichloromethane/methanol (8:2; 2×100 mL) then the organic filtrates were combined and evaporated to dryness to give the title compound as a white solid (2.25 g, 87%). LC/MS: 3.41 min; z/e 361 and 363, calcd (M−1) 361 and 363. 1H NMR (400 MHz: CDCl3): 7.40 (2H), 7.30 (5H), 7.15 (2H), 5.10 (2H), 4.05 (1H), 3.15 (1H), 2.70 (1H).

1. temperaturewas heated
2. temperatureat reflux for 3 h
3. filtrationfiltered
4. washThe filter cake was washed with dichloromethane/methanol (8:2; 2×100 mL)
5. customevaporated to dryness