HRID2417734

反应详情

EQUATION

反应方程式

HRID 2417734 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

18 g of the 4-formyl-2,4-dichlorovaleronitrile obtained in Example 3(a) and 0.1 g of copper powder are heated in a tantalum autoclave for 5 hours to 150° C. after the introduction of 10 g of dry HCl gas under pressure. After they have cooled, the contents of the autoclave are subjected to steam distillation, affording 10.5 g of 2,3-dichloro-5-methylpyridine in the form of colourless crystals with a melting point of 46°-47° C. 1H-NMR spectrum (100 MHz in CDCl3) in ppm: 8.13 (d, 1H, H on C-6); 7.59 (d, 1H, H on C-4); 2.34 (s, 3H, --CH3).

WORKUP

后处理

  1. temperatureAfter they have cooled
  2. distillationthe contents of the autoclave are subjected to steam distillation