HRID1758003

反应详情

EQUATION

反应方程式

HRID 1758003 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

To 3,4-dichlorophenol (13.8 g) dissolved in a 60 ml THF/60 ml DMSO mixture was added 9.5 g of t-BuOK. The temperature rose to about 40° C. and then 19.8 g of 2,5-bis(methylsulfonyl)pyridine was added. The reaction mixture was warmed to 50° C. and the temperature maintained at 50° C. for 1 hour. The reaction mixture was cooled, poured into approximately 3 volumes of water and the solid collected. The solid was dried on a porous plate and then recrystallized from CH2Cl2 /ethanol to give 23.5 g of 2-(3,4-dichlorophenoxy)-5-(methylsulfonyl)pyridine as shiny white plates, m.p. 120°-121° C.

WORKUP

后处理

  1. customrose to about 40° C.
  2. temperaturethe temperature maintained at 50° C. for 1 hour
  3. temperatureThe reaction mixture was cooled
  4. customthe solid collected
  5. customThe solid was dried on a porous plate
  6. customrecrystallized from CH2Cl2 /ethanol