反应详情

温度

70 °C

A solution of 2-fluoro-4-(8,8-dimethyl-5-oxo-5,6,7,8-tetrahydro-naphthalen-2-ylethynyl)benzoic acid ethyl ester (Compound 9, 0.1 g, 0.274 mmol) in ethanol(4 mL), methanol (2 mL) and tetrahydrofuran (2 mL) was treated with 1 M aqueous sodium hydroxide solution and heated at 70° C. for 1 h. The volatiles were distilled off in vacuo and the residue was diluted with water and dilute hydrochloric acid and extracted with ethyl acetate (×2). The combined organic extract was dried over anhydrous sodium sulfate, filtered and evaporated in vacuo to afford a solid that was recrystallized from hot aqueous acetonitrile to afford the title compound (0.025 g, 27%).

1. distillationThe volatiles were distilled off in vacuo
2. additionthe residue was diluted with water and dilute hydrochloric acid
3. extractionextracted with ethyl acetate (×2)
4. extractionThe combined organic extract
5. dry with materialwas dried over anhydrous sodium sulfate
6. filtrationfiltered
7. customevaporated in vacuo
8. customto afford a solid
9. customthat was recrystallized from hot aqueous acetonitrile