HRID1199915

反应详情

EQUATION

反应方程式

HRID 1199915 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

A solution of 13.77 g (72.5 mmol) of 4,6-dichloro-2-hydroxybenzaldehyde in 100 ml of DMF was stirred and 12.02 g (87 mmol) of K2CO3 was added. This mixture was heated to ~70° C. for 60 minutes, then 11.7 ml of 4-fluorobenzyl bromide was added. The resulting solution was stirred at 70° C. for 3.5 hours, then this was poured onto ice H2O (1.5 l), filtered and washed with H2O, and recrystallized from Et2O/petroleum ether. Yield: 17.88 g (83%) of off-white crystals, m.p. 107°-108° C.

WORKUP

后处理

  1. temperatureThis mixture was heated to ~70° C. for 60 minutes
  2. additionthis was poured onto ice H2O (1.5 l)
  3. filtrationfiltered
  4. washwashed with H2O
  5. customrecrystallized from Et2O/petroleum ether