HRID487033

反应详情

EQUATION

反应方程式

HRID 487033 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Into a solution of 21.23 g (50 mmol) of 2,2'-methylenebis(4,6-di-tert-butylphenol) and 7 mL (50 mmol) of triethylamine in 200 mL of toluene is added dropwise a solution of 23.84 g (50 mmol) of 3-chloro-2,4,8,10-tetra-tert-butyl-dibenzo[d,f][1,3,2]dioxaphosphepin in 100 mL of toluene at ambient temperature. After 20 hours of stirring at ambient temperature, the reaction mass is filtered to remove triethylamine hydrochloride and the filtrate is concentrated in vacuo to give a brownish oil. Trituration of the crude oil with 200 mL of acetonitrile gives 36.65 g (85% yield) of a white solid: m.p.=195°-205° C.

WORKUP

后处理

  1. filtrationthe reaction mass is filtered
  2. customto remove triethylamine hydrochloride
  3. concentrationthe filtrate is concentrated in vacuo
  4. customto give a brownish oil