反应详情

2.2.2-Trichioro-1-[10-(4-cyclohex-1-en-1-yl-3-methyl-benzoyl)-10,11-dihydro-5H-pvrrolo[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 0.450 g 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