HRID1493318

反应详情

EQUATION

反应方程式

HRID 1493318 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 26.5 g of 2-chloro-3-nitropyridine, 23.7 g of 4-chlorobenzylamine and 25 ml of 2-methyl-5-ethylpyridine in 200 ml of xylene is refluxed for 12 hours. The reaction mixture is then cooled, water and acetic acid are added and the resulting mixture is then extracted with ether. The organic phase is dried over magnesium sulfate, filtered and then evaporated under vacuum to give an oil which crystallizes from isopropyl ether. The crystals are filtered off and then dried to give 27 g of 2-(4-chlorophenylmethylamino)-3-nitropyridine in the form of crystals melting at 100° C.

WORKUP

后处理

  1. temperatureThe reaction mixture is then cooled
  2. extractionthe resulting mixture is then extracted with ether
  3. dry with materialThe organic phase is dried over magnesium sulfate
  4. filtrationfiltered
  5. customevaporated under vacuum
  6. customto give an oil which
  7. customcrystallizes from isopropyl ether
  8. filtrationThe crystals are filtered off
  9. customdried