HRID1288226

反应详情

EQUATION

反应方程式

HRID 1288226 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 2-phenoxypropylamine p-toluenesulphonate (3.7 g.) and phenylacetonitrile (1.5 g.) was stirred and heated, in an oil-bath, to 270° for 11/2 hours. The mixture was cooled and dissolved in the minimum amount of boiling ethanol, and the solution was poured into a mixture of water (75 ml.) and ether (75 ml.). The mixture was shaken and the aqueous layer was separated, washed once with ether, and evaporated to half-volume under reduced pressure. An oil separated and crystallised after a few days. The product was filtered and recrystallised from water to give N-(2-phenoxypropyl)phenylacetamidine p-toluenesulphonate, m.p. 121°-124°.

WORKUP

后处理

  1. temperatureheated, in an oil-bath, to 270° for 11/2 hours
  2. temperatureThe mixture was cooled
  3. stirringThe mixture was shaken
  4. customthe aqueous layer was separated
  5. washwashed once with ether
  6. customevaporated to half-volume under reduced pressure
  7. customAn oil separated
  8. customcrystallised after a few days
  9. filtrationThe product was filtered
  10. customrecrystallised from water