反应详情

Triethylamine (2.92 ml) was added to a mixture of 1-(6-chloronaphth-2-ylsulphonyl)piperazine hydrochloride (6.93 g) in dichloromethane (100 ml). 1-(1-(t-butoxycarbonyl)piperidin-4-ylcarbonyloxy)-2,5-dioxopyrrolidine (6.25 g) was added and the mixture stirred overnight. The mixture was evaporated to give a solid which was suspended in ethyl acetate (200 ml). Water (50 ml) was added and the ethyl acetate phase separated, washed with water (4×50 ml), brine (50 ml), dried (MgSO4) and evaporated. The residue was purified by flash chromatography on silica gel using a 75:25 mixture of ethyl acetate/hexane as eluent to give 1-(t-butoxycarbonyl)-4-(1-(6-chloronaphth-2-ylsulphonyl)piperazin-4-ylcarbonyl)piperidine (8.1 g);

1. customThe mixture was evaporated
2. customto give a solid which
3. customthe ethyl acetate phase separated
4. washwashed with water (4×50 ml), brine (50 ml)
5. dry with materialdried (MgSO4)
6. customevaporated
7. customThe residue was purified by flash chromatography on silica gel using
8. additiona 75:25 mixture of ethyl acetate/hexane as eluent