HRID652105

反应详情

EQUATION

反应方程式

HRID 652105 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Methyl N-[2-(methylthio)acetyl]-1-methyl-2-(phenylmethylene)hydrazine carboximidothioate (1.2 g) and 3-[4-(1-piperidinylmethyl)phenoxy]propanamine (0.9 g) were heated at 55° under water vacuum for 2 h. Additional carboximidothioate (0.09 g) was then added and the mixture heated for a further 1 h. The reaction mixture was dissolved in toluene (5 ml) and 5N hydrochloric acid (4 ml), stirred at room temperature for 18 h and the phases separated. The aqueous phase was basified to pH 10 with sodium carbonate and extracted with ethyl acetate to give an oil, which was chromatographed using ethyl acetate-methanol (3:1) to give the title compound (1.04 g) as an orange brown oil.

WORKUP

后处理

  1. additionAdditional carboximidothioate (0.09 g) was then added
  2. temperaturethe mixture heated for a further 1 h
  3. customthe phases separated
  4. extractionextracted with ethyl acetate
  5. customto give an oil, which
  6. customwas chromatographed