HRID232895

反应详情

EQUATION

反应方程式

HRID 232895 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A Grignard solution of p-methoxyphenylmagnesium bromide (prepared from 12.2 g (0.05 mol) of magnesium and 93.5 g (0.5 mol) of p-bromoanisole in 130 ml of anhydrous THF) is added to a solution of 31.3 g (0.17 mol) of cyanuric chloride in 100 ml of THF over a period of 1.5 hours while maintaining the temperature in the range from 0° to 20° C. After addition is complete, the mixture is stirred at room temperature for 1.5 hours and then poured into 150 ml of 12% hydrogen chloride solution in an ice-bath. The beige suspension is filtered off, washed neutral with water and then washed with methanol. The crude product is recrystallized from 350 ml of toluene to give the compound of the formula ##STR21##

WORKUP

后处理

  1. temperaturewhile maintaining the temperature in the range from 0° to 20° C
  2. additionAfter addition
  3. filtrationThe beige suspension is filtered off
  4. washwashed neutral with water
  5. washwashed with methanol
  6. customThe crude product is recrystallized from 350 ml of toluene
  7. customto give the compound of the formula