反应详情

A solution of 0.100 g (0.26 mmol) of 3-{4-[(E)-3-(3,4-dichloro-phenyl)-acryloyl]-7-oxo-[1,4]diazepan-1-yl}-propionic acid (intermediate 5) and 0.032 g (0.31 mmol) of 4-hydroxypiperidine in 5 ml of dichloromethane was treated at 0° C. with 0.060 g (0.31 mmol) of EDCI. The cooling bath was allowed to come to RT and after 4 h the reaction was extracted with aqueous 10% KHSO4/EtOAc (3×). The organic phases were washed with aqueous saturated NaHCO3, 10% NaCl and dried over Na2SO4 to yield after evaporation of the solvent 0.108 g (89%) of the titled compound as white solid. MS: 468.3 (MH+, 1Cl).

1. extractionthe reaction was extracted with aqueous 10% KHSO4/EtOAc (3×)
2. washThe organic phases were washed with aqueous saturated NaHCO3, 10% NaCl
3. dry with materialdried over Na2SO4
4. customto yield
5. customafter evaporation of the solvent 0.108 g (89%) of the titled compound as white solid