HRID1165973

反应详情

EQUATION

反应方程式

HRID 1165973 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of lactone from Example 1, part A(5) (10.05 gm, 46.31 mmole) in THF-H2O (100 ml -18 ml) was treated slowly with 1M lithium hydroxide (60 ml). The reaction was stirred at room temperature under argon for 2 hours, concentrated and acidified to pH 6 with HCl. The solution was washed several times with ethyl acetate, acidified to pH 1 with HCl, saturated with sodium chloride and extracted with ethyl acetate. The extracts were washed with brine, dried over sodium sulfate, filtered and concentrated to an oil which was crystallized from dichloromethane-hexane to afford 7.7 gm (71%) of the title compound.

WORKUP

后处理

  1. concentrationconcentrated
  2. washThe solution was washed several times with ethyl acetate
  3. extractionextracted with ethyl acetate
  4. washThe extracts were washed with brine
  5. dry with materialdried over sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated to an oil which
  8. customwas crystallized from dichloromethane-hexane