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 1.3 g of N-cyano-O-phenylisourea and 1.2 g of 1,2,3,4-tetrahydro-1-naphthylamine in 5 ml of chloroform was heated at reflux in an oil bath. Disappearance of the isourea was monitored by thin layer chromatography analysis. After 30 hours, the resulting thick solution was treated with 5 ml of toluene and allowed to stand at room temperature which resulted in the crystallization of the desired product. The supernatant solution was withdrawn and the product washed with toluene (10 ml). Upon drying under vacuum, 0.91 g of the desired compound was obtained. A second crop of crystals was collected after concentrating the mother liquor slightly. Total yield of N'-cyano-N-(1,2,3,4-tetrahydro-1-naphthyl)guanidine was 1.29 g, mp 153°-155° C.
WORKUP
后处理
- temperaturewas heated
- temperatureat reflux in an oil bath
- customto stand at room temperature