反应详情

A cooled (0° C.) solution of 0.150 g (0.29 mmol) of 2-{4-[(E)-3-(3,4-dichloro-phenyl)-acryloyl]-7-oxo-[1,4]diazepan-1-yl}-4-oxo-4-piperidin-1-yl-butyric acid methyl ester in 3.7 ml of EtOH was treated with 0.013 g (0.59 mmol) of LiBH4 (in 3 portions during 48 h until to the end of the reaction). The mixture was stirred at RT for 48 h, cooled to 0° C. and aqueous 10% KHSO4 solution was slowly added. The mixture was partitioned between aqueous saturated NaHCO3/EtOAc (3×). The organic phases were dried (Na2SO4) and evaporated to give 0.136 g (96%) of the titled compound as white foam. MS: 482.2 (MH+, 2Cl).

1. customuntil to the end of the reaction)
2. temperaturecooled to 0° C.
3. customThe mixture was partitioned between aqueous saturated NaHCO3/EtOAc (3×)
4. dry with materialThe organic phases were dried (Na2SO4)
5. customevaporated