HRID390117

反应详情

EQUATION

反应方程式

HRID 390117 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The ester 1e (2.26 g) was mixed with THF (20 ml), MeOH (20 ml) and a solution of LiOH (1N 20, ml) and stirred at 55° C. for ˜17 h. The reaction mixture was concentrated by rotary evaporation, diluted with water (30-50 ml) and acidified with 10% citric acid to pH 3-4. The cloudy solution was extracted into ethyl acetate (3×50 ml). The combined organic extracts were washed with water and brine, and dried over magnesium sulfate. The drying agent was removed by filtration and the ethyl acetate was removed by rotary evaporation. The residue was dried on high vacuum which gave 2 g of the title compound as a white foam. The product was used directly without further purification.

WORKUP

后处理

  1. concentrationThe reaction mixture was concentrated by rotary evaporation
  2. additiondiluted with water (30-50 ml)
  3. extractionThe cloudy solution was extracted into ethyl acetate (3×50 ml)
  4. washThe combined organic extracts were washed with water and brine
  5. dry with materialdried over magnesium sulfate
  6. customThe drying agent was removed by filtration
  7. customthe ethyl acetate was removed by rotary evaporation
  8. customThe residue was dried on high vacuum which