HRID438030

反应详情

EQUATION

反应方程式

HRID 438030 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 0.15 mole each of diphenyl phenylphosphonite, acetaldehyde, and p-toluenesulfonamide in 100 g of chlorobenzene is stirred and warmed at 103°-115° C. for 1 hr, and the solvent and by-product phenol are removed by concentration of the reaction mixture to 120° at 0.5 mm. Ether is stirred into the residue, causing separation of 49.4g (79% yield) of solid product. Recrystallization twice from chlorobenzene gives a white solid: mp 178°-181°; 31P nmr (DMSO-d6)- 37.7 ppm.

WORKUP

后处理

  1. temperaturewarmed at 103°-115° C. for 1 hr
  2. customthe solvent and by-product phenol are removed by concentration of the reaction mixture to 120° at 0.5 mm
  3. stirringEther is stirred into the residue