反应详情

A solution of 0.085 g (0.25 mmol) of 4-(2-chloro-ethyl)-1-[(E)-3-(3-chloro-phenyl)-acryloyl]-[1,4]diazepan-5-one in 1.3 ml of DMA was treated with 0.04 ml (0.50 mmol) of morpholine and stirred for 8 h at RT, a crystal of NaI was added and stirring was continued for 40 h. The reaction was extracted with aqueous saturated NaHCO3/EtOAc (3×). The organic phases were washed with aqueous 10% NaCl, dried (Na2SO4), concentrated and evaporated. Purification by catridges, Si-Amine, 70 ml, 20 g (EtOAc) gave 0.008 g (8%) of the title compound as off-white viscous oil. MS: 392.0 (MH+, Cl).

1. stirringstirring
2. waitwas continued for 40 h
3. extractionThe reaction was extracted with aqueous saturated NaHCO3/EtOAc (3×)
4. washThe organic phases were washed with aqueous 10% NaCl
5. dry with materialdried (Na2SO4)
6. concentrationconcentrated
7. customevaporated
8. customPurification by catridges, Si-Amine, 70 ml, 20 g (EtOAc)