HRID1074427

反应详情

EQUATION

反应方程式

HRID 1074427 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4 g=20 mmoles of 2-chloro-4-(N,N-dimethylaminomethyl)-6-methylphenol are added in portions, while cooling with an ice bath and stirring, to a suspension of 0.6 g=20 mmoles of sodium hydride (an 80% strength dispersion in oil) in 30 ml of absolute dimethylformamide at such a rate that the temperature does not exceed 20° C. Stirring is continued at 20° C. until the evolution of hydrogen is complete, 8.26 g=20 mmoles of 2-bromomethyl-2-(4-chlorophenyl)-1,3-dioxolan-4-ylmethyl methanesulfonate (compound of the formula (IV)) are then introduced in portions, stirring is continued for 7 hours at 60° C. and the mixture is worked up as described in Example 1a. This gives 7 g (71% of theory) of a highly viscous, noncrystalline oil.

WORKUP

后处理

  1. temperaturewhile cooling with an ice bath
  2. customdoes not exceed 20° C
  3. stirringstirring