反应详情

8-Fluoro-3-methoxy-12-(4-methylpiperazin-1-yl)-6H-[1]benzothieno[2,3-b][1,5]benzodiazepine (500 mg) was dissolved in dichloromethane (15 ml) and ethanedithiol (2.10 ml) and aluminium chloride (2.51 g) were added. The mixture was stirred at room temperature for 2 hours. Water (50 ml) was added to the reaction mixture and 10% aqueous sodium hydroxide solution was added until it assumed alkaline. The mixture was extracted with chloroform, washed with water, washed with saturated aqeuous sodium chloride solution and dried over sodium sulfate. The solvent was evaporated under reduced pressure, and the residue was separated by silica gel column chromatography (chloroform:methanol=5:1) and recrystallized from ethyl acetate to give 8-fluoro-3-hydroxy-12-(4-methylpiperazin-1-yl)-6H-[1]benzothieno[2,3-b][1,5]benzodiazepine (251 mg).

1. additionwas added until it
2. extractionThe mixture was extracted with chloroform
3. washwashed with water
4. washwashed with saturated aqeuous sodium chloride solution
5. dry with materialdried over sodium sulfate
6. customThe solvent was evaporated under reduced pressure
7. customthe residue was separated by silica gel column chromatography (chloroform:methanol=5:1)
8. customrecrystallized from ethyl acetate