HRID1288226
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureheated, in an oil-bath, to 270° for 11/2 hours
- temperatureThe mixture was cooled
- stirringThe mixture was shaken
- customthe aqueous layer was separated
- washwashed once with ether
- customevaporated to half-volume under reduced pressure
- customAn oil separated
- customcrystallised after a few days
- filtrationThe product was filtered
- customrecrystallised from water