HRID75124

反应详情

EQUATION

反应方程式

HRID 75124 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 Intermediate 3-2 (4.21 g) and TEA (2.0 g) in DCM (50 mL) was added benzoyl chloride (2.11 g) slowly. After stirring at room temperature for 1 hour and then the reaction was quenched with saturated sodium bicarbonate. The organic phase was dried over sodium sulfate and evaporated to dryness. Purification was achieved by chromatography on an ISCO column (RediSep 12, gradient elution with 10% to 70% EtOAc/Hex providing pure Intermediate 3-3 (2.82 g, 49% yield for the three steps).

WORKUP

后处理

  1. customthe reaction was quenched with saturated sodium bicarbonate
  2. dry with materialThe organic phase was dried over sodium sulfate
  3. customevaporated to dryness
  4. customPurification
  5. washRediSep 12, gradient elution with 10% to 70% EtOAc/Hex