HRID1388280

反应详情

EQUATION

反应方程式

HRID 1388280 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
40 °C

PROCEDURE

实验过程

7.73 g of 30% aqeous glyoxal solution (40 mmols glyoxal), 16.17 g (80 mmols) of diphenylphosphine oxide and 40 ml of benzene were introduced into a round bottom flask. The initial pH of the reaction mixture was heated for 30 min with a water bath at 40° C. The precipitated white product was separated by filtration and weighed 16.64 g (90% yield) m.p. 211°-214° C. After recrystallization from dimethylsulfoxide-acetonitrile 3:2, V:V gave a sample of 1,2-dihydroxy-1,2-bis(diphenylphosphinyl)ethane m.p. 216°-217° C. Anal. Calcd for C26H24O4P2 : C,67.53; H, 5.23. Found: C,67.42; H, 5.34.

WORKUP

后处理

  1. customThe precipitated white product was separated by filtration
  2. customAfter recrystallization from dimethylsulfoxide-acetonitrile 3:2, V