HRID1165964

反应详情

EQUATION

反应方程式

HRID 1165964 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of Part A (cis)-1-benzoyl-4-fluoro-L-proline methyl ester (3.7 g, 14.74 mmole) in tetrahydrofuran-water (37 ml-7 ml) was added 31 ml of a 1N solution of lithium hydroxide in water. The reaction was stirred at room temperature for 2 hours. The tetrahydrofuran was evaporated, the pH of the residual aqueous solution was adjusted to 8 and extracted with ethyl acetate. The organic extracts were discarded. The aqueous phase was acidified to pH 2 with concentrated HCl and extracted with dichloromethane. The organic extracts were washed with brine and dried (sodium sulfate). The organic solution was filtered and concentrated to 2.9 g of solid.

WORKUP

后处理

  1. customThe tetrahydrofuran was evaporated
  2. extractionextracted with ethyl acetate
  3. extractionextracted with dichloromethane
  4. washThe organic extracts were washed with brine
  5. dry with materialdried (sodium sulfate)
  6. filtrationThe organic solution was filtered
  7. concentrationconcentrated to 2.9 g of solid