反应详情

A solution of lithium hydroxide (1.63 g, 0.068 mole) in water (70 ml) was added to a solution of the product of Step A (7.6 g, 0.021 mole) in ethylene glycol dimethyl ether (100 ml) with cooling in an ice bath. The reaction mixture was stirred at room temperature under Ar for 2 hours, concentrated in vacuo, and extracted (2×) with ethyl acetate. The aqueous phase was neutralized with 10% of citric acid, cooled and filtered to give the product as a white solid (6.6 g), mp >193° (dec).

1. temperaturewith cooling in an ice bath
2. concentrationconcentrated in vacuo
3. extractionextracted (2×) with ethyl acetate
4. temperaturecooled
5. filtrationfiltered