反应详情

温度

50 °C

A solution of ethyl 2-[4-(acetyloxy)-2-methylphenoxy]-2-methylpropanoate (intermediate 9, 40.8 g) in ethanol (280 ml) was treated with sodium ethoxide (12.9 g) at room temperature under nitrogen. The resulting solution was heated to 50° C. for 1 hour. 2M hydrochloric acid (95 ml) was added to the cooled reaction and the solution concentrated. The residue was dissolved in t-butylmethyl ether and the resulting solution washed with water followed by brine and then dried over sodium sulfate, filtered and the filtrate concentrated to give a brown oil. Further purification by Biotage® chromatography eluting initially with cyclohexane and then cyclohexane:ethyl acetate (5:1) gave the title compound as an orange oil.

1. concentrationthe solution concentrated
2. dissolutionThe residue was dissolved in t-butylmethyl ether
3. washthe resulting solution washed with water
4. dry with materialdried over sodium sulfate
5. filtrationfiltered
6. concentrationthe filtrate concentrated
7. customto give a brown oil
8. customFurther purification by Biotage® chromatography
9. washeluting initially with cyclohexane