反应详情

温度

55 °C

A solution of [4-(2,2,4,4-tetramethyl-chroman-6-yl-ethynyl)phenyl]acetic acid methyl ester (Compound 27, 0.047 g, 0.13 mmol) in 5 mL of methanol was treated with 1M sodium hydroxide solution (2 mL) and heated at 55° C. for 2 h. The volatiles were distilled off in vacuo and the residue was acidified with 10% hydrochloric acid and extracted with ethyl acetate (×2). The combined organic phase was washed with brine (×1), dried over anhydrous sodium sulfate, filtered and evaporated in vacuo to a residue which was purified by preparative reverse phase HPLC using 10% water in acetonitrile as the mobile phase to afford the title compound (0.034 g, 82%).

1. distillationThe volatiles were distilled off in vacuo
2. extractionextracted with ethyl acetate (×2)
3. washThe combined organic phase was washed with brine (×1)
4. dry with materialdried over anhydrous sodium sulfate
5. filtrationfiltered
6. customevaporated in vacuo to a residue which
7. customwas purified by preparative reverse phase