反应详情

To a solution of 10-[(4-bromophenyl)sulfonyl]-10,11-dihydro-5H-pyrrolo[2,1-c][1,4]benzodiazepine of Step A (2.32 g, 5.753 mmol) and N,N-dimethylaniline (1.17 mL, 9.204 mmol) in dry dichloromethane (20 mL) at 0° C. under nitrogen was added dropwise trichloroacetyl chloride (0.96 mL, 8.629 mmol). The ice bath was removed and the reaction mixture stirred at room temperature for 21 hours. The reaction mixture was then washed with 2 M hydrochloric acid (2×100 mL) and water (100 mL), dried over anhydrous magnesium sulfate, and concentrated in vacuo to give an olive foam. Purification by flash chromatography using a solvent gradient of 5-15% ethyl acetate in hexane afforded a cream solid that was recrystallized from diethyl ether/hexane to afford the title compound (1.986 g, 63%) as an off-white crystalline solid, m.p. 182-183 ° C.

1. customThe ice bath was removed
2. washThe reaction mixture was then washed with 2 M hydrochloric acid (2×100 mL) and water (100 mL)
3. dry with materialdried over anhydrous magnesium sulfate
4. concentrationconcentrated in vacuo
5. customto give an olive foam
6. customPurification by flash chromatography
7. customafforded a cream solid
8. customthat was recrystallized from diethyl ether/hexane