反应详情

The carboxylate (3a) (4 g, 19.49 mmol, 1 eq) obtained in (2-1) was added to aqueous solution of sodium hydroxide (2M, 98 mL, 0.20 mmol, 10 eq). The suspension was stirred and heated until the reaction mixture was uniform, and then refluxed for 30 minutes with heating. The mixture solution was acidified, and the resulting precipitate was extracted three times with ethyl acetate (100 mL). The extracts were combined, washed with water, dried over magnesium sulfate, and concentrated to give white solid of the title compound (4a) (3.71 g, yield 99%).

1. temperatureheated until the reaction mixture
2. temperaturerefluxed for 30 minutes
3. temperaturewith heating
4. extractionthe resulting precipitate was extracted three times with ethyl acetate (100 mL)
5. washwashed with water
6. dry with materialdried over magnesium sulfate
7. concentrationconcentrated