HRID35059

反应详情

EQUATION

反应方程式

HRID 35059 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 1-methyl-3-chloro-N5 -[3-[3-[(dimethylamino)methyl]phenoxy]propyl]-1H-1,2,4-triazole-5-amine (0.4 g), pyrrolidine (0.71 g) and sodium iodide (0.3 g) was heated at 180° in an autoclave for 16 hr. The reaction mixture was dissolved in dilute hydrochloric acid, washed with ethyl acetate, basified with sodium hydroxide and extracted with toluene. The toluene extracts were fractionally distilled to give the title compound as a pale yellow oil (0.27 g) b.p. 210° (0.04 mm). TLC silica; ethyl acetate:isopropanol:water:0.88 ammonia 25:15:8:2; Rf 0.6.

WORKUP

后处理

  1. temperaturewas heated at 180° in an autoclave for 16 hr
  2. washwashed with ethyl acetate
  3. extractionextracted with toluene
  4. distillationThe toluene extracts were fractionally distilled