HRID2047477

反应详情

EQUATION

反应方程式

HRID 2047477 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of the compound (5.2 g) obtained in step 1 in THF/methanol/water (6.0/18/9.5 mL) was added 4N aqueous lithium hydroxide solution (9.5 mL), and the mixture was stirred at room temperature for 4 hr. The mixture was acidified with 1N hydrochloric acid, concentrated under reduced pressure, diluted with water, and extracted with ethyl acetate. The extract was washed with water and saturated brine, dried, filtered through silica gel (eluted with ethyl acetate). The filtrate was concentrated under reduced pressure, and crystallized from ethyl acetate/hexane to give the title compound (4.3 g, 86%) as a pale-yellow powder.

WORKUP

后处理

  1. concentrationconcentrated under reduced pressure
  2. additiondiluted with water
  3. extractionextracted with ethyl acetate
  4. washThe extract was washed with water and saturated brine
  5. customdried
  6. filtrationfiltered through silica gel (eluted with ethyl acetate)
  7. concentrationThe filtrate was concentrated under reduced pressure
  8. customcrystallized from ethyl acetate/hexane