反应详情

A suspension of methyl 3,3-bis(4-chlorophenyl)propenoate (Step A, 3.0 g, 14 mmol) and platinum dioxide (0.30 g) in MeOH (20 mL) and 2 M aqueous hydrochloric acid (1 mL) was degassed and filled with hydrogen with a balloon. After stirring at room temperature for 2 h, the reaction mixture was filtered through CELITE diatomaceous earth, and the filtrate was concentrated to dryness. The residue was dissolved in 50 mL ether and was concentrated with 20 g silica gel. The material was loaded onto a silica gel column, which was eluted with 10% ether in hexane to give the title compound. 1H NMR (500 MHz, CD3OD): δ 7.29-7.22 (m, 4H), 4.50 (t, 1H), 3.56 (s, 3H), 3.07 (d, 2H). LC-MS: m/e 309 (M+H)+ (4.1 min).

1. customwas degassed
2. additionfilled with hydrogen with a balloon
3. filtrationthe reaction mixture was filtered through CELITE diatomaceous earth
4. concentrationthe filtrate was concentrated to dryness
5. dissolutionThe residue was dissolved in 50 mL ether
6. concentrationwas concentrated with 20 g silica gel
7. washwas eluted with 10% ether in hexane