反应详情

Mixture of isomer A of 4-((3,5-bis(trifluoromethyl)benzyloxy)methyl)-4-phenylazepane (3 mg) and acetone (1.2 mg) in methanol (0.15 mL) was stirred at room temperature for 0.5 hr, then sodium cyanoborohydride (1.0 M solution in THF, 0.02 mL) was added followed by 1 drop of trifluoroacetic acid. The mixture was stirred at 65° C. for overnight and concentrated under vacuum. Then saturated sodium bicarbonate solution and dichloromethane was added to the mixture and the organic layer was separated. The aqueous layer was extracted with dichloromethane 2 times and the combined organic layers were dried over magnesium sulfate, filtered and concentrated under vacuum to give the product as a clear sticky oil (2.5 mg, 76% yield).

1. stirringThe mixture was stirred at 65° C. for overnight
2. concentrationconcentrated under vacuum
3. additionThen saturated sodium bicarbonate solution and dichloromethane was added to the mixture
4. customthe organic layer was separated
5. extractionThe aqueous layer was extracted with dichloromethane 2 times
6. dry with materialthe combined organic layers were dried over magnesium sulfate
7. filtrationfiltered
8. concentrationconcentrated under vacuum