反应详情

A suspension of (6-bromo-1,2-benzisoxazol-3-yl)acetic acid (Intermediate 32) (0.06 g) and HATU (0.09 g) in dry tetrahydrofuran (2 ml) was stirred at room temp. for 5 min. 1-Hydroxybenzotriazole (0.03 g) and 1,1-dimethylethyl 1-piperazinecarboxylate (0.04 g) were added and the reaction mixture was stirred for a further 18 h. The solvent was removed under vacuum and the residue was partitioned between dichloromethane and 2N aqueous sodium carbonate. The layers were separated and the organic layer was applied to a Varian Bond-Elut SPE cartridge (silica, 5 g ) eluting sequentially with dichloromethane, chloroform, ether and ethyl acetate to give the title compound as a white solid (0.09 g).

1. stirringthe reaction mixture was stirred for a further 18 h
2. customThe solvent was removed under vacuum
3. customthe residue was partitioned between dichloromethane and 2N aqueous sodium carbonate
4. customThe layers were separated
5. washeluting sequentially with dichloromethane, chloroform, ether and ethyl acetate