反应详情

温度

160 °C

Intermediate 60 (2.6 g, 16.54 mmol) was dissolved in ethyleneglycol and added potassium hydroxide (5.6 g, 99.2 mmol). This mixture was heated to 160° C. for 2 h. After two hours reaction mixture was cooled to rt and toluene and water were added. Aqueous layer separated and acidified with HCl and pH adjusted to 4. Aqueous layer extracted with ethyl acetate and ethyl acetate layer was dried on anhydrous sodium sulphate. Ethyl acetate removed on rotavapour to obtain the title compound (930 mg) as a white solid.

1. customAfter two hours reaction mixture
2. temperaturewas cooled to rt
3. customAqueous layer separated
4. extractionAqueous layer extracted with ethyl acetate and ethyl acetate layer
5. dry with materialwas dried on anhydrous sodium sulphate
6. customEthyl acetate removed on rotavapour