反应详情

To an ice-cooled solution of 2.13 g (3.50 mmol) of 1-[(E)-3-(3-chloro-phenyl)-acryloyl]-4-(2-hydroxy-ethyl)-[1,4]diazepan-5-one and 0.73 ml (5.25 mmol) of Et3N in 35 ml of dichloromethane were added 0.29 ml (3.68 mmol) of methanesulfonyl chloride under stirring within 5 min keeping the temperatue at 0° C. The reaction was stirred at room temperature for 1 h 45 min. Water was added and after 5 min, the reaction was then partitioned between ether and aqueous saturated NaHCO3. The water phase was extracted again with ether (2×), the organic phases were washed with aqueous 10% NaCl, dried (Na2SO4) and concentrated to yield 1.22 g (87%) of the title compound as yellow viscous oil. MS: 341.0 (MH+, 2Cl).

1. customat 0° C
2. stirringThe reaction was stirred at room temperature for 1 h 45 min
3. customthe reaction was then partitioned between ether and aqueous saturated NaHCO3
4. extractionThe water phase was extracted again with ether (2×)
5. washthe organic phases were washed with aqueous 10% NaCl
6. dry with materialdried (Na2SO4)
7. concentrationconcentrated