反应详情

NBS (3.12 g) was added portionwise over 1 hour to a solution of 2-(3,5-dimethylphenyl)acetic acid (3.6 g) and AIBN (0.015 g) in ethyl acetate (100 mL) at 50° C. under nitrogen. More AIBN (0.015 g) was added and the mixture was heated to reflux for 3 hours. The reaction mixture was washed with 10% aqueous sodium chloride solution (2×200 mL), dried over magnesium sulphate, filtered and evaporated. The crude material was purified by flash silica chromatography using 20% ethyl acetate in isohexane containing 1% acetic acid as solvent. Fractions containing the product were evaporated to dryness to afford a solid which was triturated with cyclohexane (10 mL) to yield the subtitled compound as a white solid. Yield 2.10 g.

1. temperaturethe mixture was heated
2. temperatureto reflux for 3 hours
3. washThe reaction mixture was washed with 10% aqueous sodium chloride solution (2×200 mL)
4. dry with materialdried over magnesium sulphate
5. filtrationfiltered
6. customevaporated
7. customThe crude material was purified by flash silica chromatography
8. additionFractions containing the product
9. customwere evaporated to dryness
10. customto afford a solid which
11. customwas triturated with cyclohexane (10 mL)