反应详情

177 μl of triethylamine (1.27 mmol) and 15.5 mg of DMAP (0.127 mmol) were added to a solution of the amine hydrochloride from Example 62A (200 mg, 0.422 mmol) in dichloromethane (10 ml), and 84 mg of cyclopentanecarbonyl chloride (0.633 mmol) were then added at 0° C. The reaction mixture was warmed to RT and stirred overnight. The reaction solution was washed with aqueous 1 N hydrogen chloride solution and the organic phase was dried over magnesium sulphate, filtered and concentrated under reduced pressure. The crude product was purified by preparative HPLC (RP18 column; acetonitrile/water gradient). Yield: 112 mg (52% of theory)

1. additionwere then added at 0° C
2. washThe reaction solution was washed with aqueous 1 N hydrogen chloride solution
3. dry with materialthe organic phase was dried over magnesium sulphate
4. filtrationfiltered
5. concentrationconcentrated under reduced pressure
6. customThe crude product was purified by preparative HPLC (RP18 column; acetonitrile/water gradient)