反应详情

To a solution of 3a in methanol (0.2 M) was added palladium, 10 weight % (dry basis) on activated carbon, wet, (0.1 eq) and concentrated hydrochloric acid (3.5 eq). The reaction mixture was shaken overnight on a Parr reactor, with hydrogen pressure equal to 70 psi. The reaction mixture was filtered through celite, concentrated in vacuo then triturated with ether. The product was obtained as a white solid. (85%) 1H NMR (300 MHz, DMSO-d6) δ 8.66 (br s, 2H), 7.55 (m, 1H), 7.32 (m, 3H), 4.01 (m, 2H), 3.89 (s, 2H), 3.61 (s, 3H).

1. dry with materialpalladium, 10 weight % (dry basis) on activated carbon
2. filtrationThe reaction mixture was filtered through celite
3. concentrationconcentrated in vacuo
4. customthen triturated with ether
5. customThe product was obtained as a white solid