反应详情

3-[4-(10,11-Dihydro-5H-pyrrolo[2,1-c][1,4]benzodiazepine-10-carbonyl)-phenyl]-cyclohex-2-enone of Example 24 (0.100 g, 0.261 mmol) and cerium (III) chloride (0.064 g, 0.261 mmol) were dissolved in methanol (1.3 mL) followed by addition of solid sodium borohydride (0.010 g, 0.261 mmol). After hydrogen evolution ceased (approximately 5 minutes), 0.1 N hydrochloric acid (50 mL) was added and the resulting mixture extracted with ethyl acetate. The extract was dried over anhydrous magnesium sulfate, filtered and concentrated. A slightly yellow solid was isolated which was dissolved in boiling diethyl ether and filtered. The product was precipitated from the filtrate by addition of pentane and the precipitate filtered and dried to afford the title compound (0.100 g) as an amorphous white solid.

1. additionwas added
2. extractionthe resulting mixture extracted with ethyl acetate
3. dry with materialThe extract was dried over anhydrous magnesium sulfate
4. filtrationfiltered
5. concentrationconcentrated
6. customA slightly yellow solid was isolated which
7. dissolutionwas dissolved
8. filtrationfiltered
9. customThe product was precipitated from the filtrate by addition of pentane
10. filtrationthe precipitate filtered
11. customdried