反应详情

A solution of 0.286 g (0.65 mmol) of 2-{4-[(E)-3-(3,4-dichloro-phenyl)-acryloyl]-7-oxo-[1,4]diazepan-1-yl}-succinic acid 1-methyl ester (intermediate 7) in 15 ml of dichloromethane was treated with 0.070 ml (0.71 mmol) of piperidine and at 0° C. with 0.148 g (0.77 mmol) of EDCI and 0.009 g (0.06 mmol) of HOBT. Over night, the suspension was naturally warmed to RT, poured on aqueous 10% KHSO4 solution and extracted with EtOAc (3×). The organic phases were washed with aqueous saturated NaHCO3 and aqueous 10% NaCl, dried (Na2SO4) and evaporated to give 0.332 g (quant.) of the titled compound as white foam. MS: 510.1 (MH+, 2Cl).

1. waitOver night
2. extractionextracted with EtOAc (3×)
3. washThe organic phases were washed with aqueous saturated NaHCO3 and aqueous 10% NaCl
4. dry with materialdried (Na2SO4)
5. customevaporated