反应详情

A solution of 2,2,2-trichloro-1-{10-[(2′-methyl-1,1′-biphenyl-4-yl)carbonyl]-10,11-dihydro-5H-pyrrolo[2,1-c][1,4]benzodiazepine-3-yl}ethanone (1.72 mmol), and 3-aminomethylpyridine (3.44 mmol) in dimethylsulfoxide (8.6 mmol) and acetonitrile (15 mL) was stirred at 80° C. for 18 hours. The solvent was evaporated and the residue dissolved in dichloromethane, washed with water, dried over anhydrous sodium sulfate, and evaporated. The material was purified by HPLC (Normal phase, Luna CN bonded packing) and crystallized from ethyl acetate/hexane. (0.68 g; 77%), m.p. 176-177° C.

1. customThe solvent was evaporated
2. dissolutionthe residue dissolved in dichloromethane
3. washwashed with water
4. dry with materialdried over anhydrous sodium sulfate
5. customevaporated
6. customThe material was purified by HPLC (Normal phase, Luna CN bonded packing)
7. customcrystallized from ethyl acetate/hexane