反应详情

A suspension of 4.00 g (12.77 mmol) of 1-[(E)-3-(3,4-dichloro-phenyl)-acryloyl]-[1,4]diazepan-5-one and 1.63 ml (12.77 mmol) of ethyl 3-bromopropionate in 60 ml of DMF was treated at 0° C. with 0.61 g (14.05 mmol) of NaH (55% in oil) in two portions. The suspension was stirred after 30 min at RT to get a solution and further stirred over night at 0° C. The reaction was neutralized with cold aqueous 10% KHSO4 and extracted with EtOAc (3×). The organic phases were washed with aqueous 10% NaCl, dried over Na2SO4 evaporated and crystallized (dichloromethane/MeOH) to yield 3.71 g (70%) of the titled compound as an off-white solid. MS: 413.1 (MH+, 2Cl).

1. customto get a solution
2. stirringfurther stirred over night at 0° C
3. extractionextracted with EtOAc (3×)
4. washThe organic phases were washed with aqueous 10% NaCl
5. dry with materialdried over Na2SO4
6. customevaporated
7. customcrystallized (dichloromethane/MeOH)