反应详情

To a stirred suspension of 4-[(tert-butoxycarbonyl)amino]-1-methyl-1H-imidazole-2-carboxylic acid (724 mg, 3.0 mmol) in DMF (6 mL) is added TBTU (1.16 g, 3.6 mmol). After 15 min cyclopentylamine (0.44 mL, 4.5 mmol) is added. After 20 h an additional portion of cyclopentylamine (0.44 mL, 4.5 mmol) is added, and stifling continued for a further 24 h. The mixture is diluted with EtOAc and washed in turn with 1M aqueous NaHSO4, Na2CO3 and brine. The organic layer is dried (MgSO4) and evaporated. The crude material is purified by column chromatography using a gradient of 10-100% EtOAc/heptane to afford the title compound (345 mg, 37%).

1. washwashed in turn with 1M aqueous NaHSO4, Na2CO3 and brine
2. dry with materialThe organic layer is dried (MgSO4)
3. customevaporated
4. customThe crude material is purified by column chromatography