HRID1643283

反应详情

EQUATION

反应方程式

HRID 1643283 的结构方程式

PROCEDURE

实验过程

To a solution of (5)-2((R)-2-(4-fluoro-3-methylphenyl)-2-methoxyethyl)pent-4-enoic acid in 5 mL methanol was added concentrated H2SO4 (50 mL) at room temperature and the resulting solution stirred for 16 h. The reaction mixture was concentrated under reduced pressure, the residue treated with water, and the mixture was extracted with ethyl acetate (3×20 mL). The combined organic layers were washed with brine (2×10 mL) and dried over Na2SO4. The product was isolated by flash column chromatography eluting with 0% to 10% ethyl acetate/hexane gradient solvent to give 122 mg of the title compound as a colorless oil.

WORKUP

后处理

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. additionthe residue treated with water
  3. extractionthe mixture was extracted with ethyl acetate (3×20 mL)
  4. washThe combined organic layers were washed with brine (2×10 mL)
  5. dry with materialdried over Na2SO4
  6. customThe product was isolated by flash column chromatography
  7. washeluting with 0% to 10% ethyl acetate/hexane gradient solvent