HRID1276506

反应详情

EQUATION

反应方程式

HRID 1276506 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 89 mg of methyl ester (from Example 104, Step B) in 1.5 mL EtOH was added 1.0 mL of 0.5N NaOH. After 36 h the reaction was concentrated under vacuum. The residue was dissolved in 25 mL H2O and washed with 25 mL Et2O. After separating layers, the aqueous phase was acidified to pH 2 using 0.5N KHSO4. The aqueous phase was extracted with 3×25 mL of CH2Cl2. The combined extracts were dried over Na2SO4 and concentrated under vacuum to give 58 mg of a white foam which was taken on without further purification.

WORKUP

后处理

  1. concentrationAfter 36 h the reaction was concentrated under vacuum
  2. dissolutionThe residue was dissolved in 25 mL H2O
  3. washwashed with 25 mL Et2O
  4. customAfter separating layers
  5. extractionThe aqueous phase was extracted with 3×25 mL of CH2Cl2
  6. dry with materialThe combined extracts were dried over Na2SO4
  7. concentrationconcentrated under vacuum