HRID486366

反应详情

EQUATION

反应方程式

HRID 486366 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
65 °C

PROCEDURE

实验过程

A mixture of 85 g of 6-chloro-3-pyridinecarbinol, 800 ml of dioxan and 129.8 g of 3,4-dihydro-2H-pyran was treated with 5.7 g of p-toluenesulphonic acid monohydrate, stirred at room temperature for 0.75 hours and subsequently at 65° C. for 2.75 hours. The reaction mixture was treated with 15 ml of triethylamine and, after cooling, taken up in diethyl ether. Repeated washing with saturated sodium chloride solution, drying over sodium sulphate and evaporation yielded 153.2 g of crude 2-chloro-5-[(tetrahydro-2-pyranyloxy)methyl]pyridine as a brown-red oil.

WORKUP

后处理

  1. temperatureafter cooling
  2. washRepeated washing with saturated sodium chloride solution
  3. dry with materialdrying over sodium sulphate and evaporation