HRID132690

反应详情

EQUATION

反应方程式

HRID 132690 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 compound 2A (6.20 g, 26.7 mmol) in MeOH (100 mL) was treated with saturated aqueous LiOH (15 mL), and the reaction mixture was stirred at rt overnight (˜16 h). The resulting mixture was concentrated in vacuo to dryness and partitioned between a mixed solvent (50% Et2O:50% EtOAc) and H2O. The H2O layer was acidified to pH 2-3 and extracted with EtOAc (3×20 mL). The EtOAc was dried over Na2SO4 and concentrated in vacuo to give a yellow solid (2.1 g) in 38% yield.

WORKUP

后处理

  1. concentrationThe resulting mixture was concentrated in vacuo to dryness
  2. custompartitioned between a mixed solvent (50% Et2O:50% EtOAc) and H2O
  3. extractionextracted with EtOAc (3×20 mL)
  4. dry with materialThe EtOAc was dried over Na2SO4
  5. concentrationconcentrated in vacuo