HRID1287965

反应详情

EQUATION

反应方程式

HRID 1287965 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
178 °C

PROCEDURE

实验过程

A mixture of diphenylphosphine chloride (11 g, 0.05 mol), allyl alcohol (2.9 g, 0.05 mol) in 50 ml of anhydrous ether is stirred at room temperature while slowly adding pyridine (4.0 g, 0.05 mol) to it. After 40 minutes, the pyridine hydrochloride is filtered off and the ether removed by distillation. The liquid residue is heated to 150°, whereupon an exothermic reactions sets in raising the temperature quickly to 178° C. The material is then distilled, b.p. 168°-175° C/0.4 mm, whereupon it crystallizes, m.p. 108° identical to the allyl diphenylphosphine oxide made by oxidation of the phosphine. Allyl diphenylphosphine oxide prepared by this method is reported; b.p. 200°-202° C/2 mm; m.p. 94°-96° C.

WORKUP

后处理

  1. filtrationthe pyridine hydrochloride is filtered off
  2. customthe ether removed by distillation
  3. temperatureThe liquid residue is heated to 150°, whereupon an exothermic reactions sets
  4. distillationThe material is then distilled
  5. customb.p. 168°-175° C/0.4 mm, whereupon it crystallizes
  6. customAllyl diphenylphosphine oxide prepared by this method