HRID1074428

反应详情

EQUATION

反应方程式

HRID 1074428 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2.8 g=10 mmoles of 4-(4-acetylpiperazin-1-ylmethyl)-2-chloro-6-methylphenol are added in portions, while cooling and stirring, to a suspension of 0.3 g=10 mmoles of sodium hydride (an 80% strength dispersion in oil) in 20 ml of dimethylacetamide at such a rate that the temperature does not exceed 20° C. 4.1 g=10 mmoles of 2-bromomethyl-2-(4-chlorophenyl)-1,3-dioxolan-4-ylmethyl methanesulfonate are then introduced in portions and stirring is continued for 6 hours at 80° C. 0.8 g=5 mmoles of potassium iodide and 0.9 g=10 mmoles of the sodium salt of imidazole are introduced at this temperature and the mixture is then stirred for 48 hours at 160° C. and worked up as described in Example 1a. This gives 2 g (35% of theory) of a highly viscous, non-crystalline oil.

WORKUP

后处理

  1. temperaturewhile cooling
  2. customdoes not exceed 20° C
  3. stirringthe mixture is then stirred for 48 hours at 160° C.