HRID2289694

反应详情

EQUATION

反应方程式

HRID 2289694 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3.9 mL of a 1 M solution of diisobutyl aluminum hydride in dichloromethane was added to a solution of 3,5-Diisopropyl-4-{[(2,4,6-triisopropyl-phenyl)-acetyl]sulfamoyloxy}-benzoic acid methyl ester (1.0 g, 1.8 mmol) in 125 mL dichloromethane at -78° C. After 3 hours, the reaction was warmed to room temperature and then quenched with a saturated aqueous sodium sulfate solution. The reaction mixture was filtered through a pad of celite, and the filtrate was concentrated to give a white foam. Triturated with 10% diethyl ether/hexanes to give 0.29 g of the title compound as a white solid; mp 163-168° C.

WORKUP

后处理

  1. customquenched with a saturated aqueous sodium sulfate solution
  2. filtrationThe reaction mixture was filtered through a pad of celite
  3. concentrationthe filtrate was concentrated
  4. customto give a white foam
  5. customTriturated with 10% diethyl ether/hexanes