反应详情

2,2,2-Trichloro-1-[10-(4-cyclohex-1-en-1-yl-3-methyl-benzoyl)-10,11-dihydro-5H-pyrrolo[2,1-c][1,4]benzodiazepin-3-yl]-ethanone of Step D (0.700 g, 1.33 mmol), was dissolved in acetone (8.9 mL) followed by addition of 2.5 N sodium hydroxide (1.60 mL, 3.99 mmol). The reaction was stirred at room temperature for 3 hours, and acidified with 2 N hydrochloric acid. The acidic mixture was extracted with diethyl ether and the organic phase extracted with 1 N sodium hydroxide. The combined basic extracts were acidified with 2 N hydrochloric acid, and extracted with diethyl ether. The extract was dried over anhydrous sodium sulfate, filtered and concentrated. The residue was recrystallized from diethyl ether to afford 450 mg of the title compound as white crystals, 193° C. (dec.)

1. extractionThe acidic mixture was extracted with diethyl ether
2. extractionthe organic phase extracted with 1 N sodium hydroxide
3. extractionextracted with diethyl ether
4. dry with materialThe extract was dried over anhydrous sodium sulfate
5. filtrationfiltered
6. concentrationconcentrated
7. customThe residue was recrystallized from diethyl ether