反应详情

10% Palladium-on-carbon (0.3 g) was added to a solution of 2,2-diphenyl-5-[N-(4-cyanophenethyl)-N-methylamino]pentanamide (0.3 g-see Example 13) in 5% formic acid in methanol (21 ml). The mixture was stirred at room temperature under nitrogen for 1 hour, then filtered and the filtrate concentrated in vacuo to give a gum which was purified by column chromatography on silica eluting with dichloromethane containing methanol (2% up to 10%). The product-containing fractions were combined and concentrated in vacuo to give an oil which crystallised on standing. The solid was triturated with ether to give the title compound as buff crystals, yield 0.1 g, m.p. 139°-142°.

1. filtrationfiltered
2. concentrationthe filtrate concentrated in vacuo
3. customto give a gum which
4. customwas purified by column chromatography on silica eluting with dichloromethane
5. additioncontaining methanol (2% up to 10%)
6. concentrationconcentrated in vacuo
7. customto give an oil which
8. customcrystallised
9. customThe solid was triturated with ether