HRID1195446

反应详情

EQUATION

反应方程式

HRID 1195446 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

334 g (1 mol) of 2-(4-hydroxyphenyl)-2-(4-methylphenyl)hexafluoropropane, 1.2 dm3 of dimethylacetamide, 200 cm3 of toluene and 44 g of sodium hydroxide were refluxed until it was no longer possible to separate off any water of reaction using a water separator. The toluene was then removed by distillation, 164.4 g (1.1 mol) of 4-chloronitrobenzene were added, and the mixture was refluxed for 48 hours. After the mixture had been cooled to about 0° C., the solid was filtered off, washed with about 100 cm3 of dimethylacetamide and discarded. As much of the dimethylacetamide as possible was removed from the filtrate by vacuum distillation. The oily residue was taken up in 800 cm3 of methanol, a yellow solid precipitating out. The solid was separated off and dried. After the mother liquor had been worked up, a total of 325 g (71% of theory) of a yellow solid were obtained.

WORKUP

后处理

  1. customto separate off
  2. customany water of reaction
  3. additionwere added
  4. temperaturethe mixture was refluxed for 48 hours
  5. filtrationthe solid was filtered off
  6. washwashed with about 100 cm3 of dimethylacetamide
  7. customAs much of the dimethylacetamide as possible was removed from the filtrate by vacuum distillation
  8. customa yellow solid precipitating out
  9. customThe solid was separated off
  10. customdried
  11. customa total of 325 g (71% of theory) of a yellow solid were obtained