HRID2163934

反应详情

EQUATION

反应方程式

HRID 2163934 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Lead cyanamide (24.7 g.) was added to a solution of N-methyl-N'-[2-(4-imidazolylmethylthio)ethyl]thiourea (11.5 g.) in acetonitrile (250 ml.) containing demethylformamide. The stirred suspension was heated under reflux for 48 hours. Filtration followed by concentration under reduced pressure and purification of the product on a column of silica gel with ethyl acetatle-isopropyl alcohol (2.1) as eluant gave N-cyano-N'-[2-(4-imidazolylmethylthio)ethyl]-N"-methylguanidine (3.7 g.), m.p. 138°-140° (from acetonitrile). (Found: C, 45.7; H, 5.9; N, 35.5; S, 13.5. 9H14N6S requires: C, 45.4; H, 5.9; N, 35.3; S, 13.5).

WORKUP

后处理

  1. temperatureThe stirred suspension was heated
  2. temperatureunder reflux for 48 hours
  3. filtrationFiltration
  4. concentrationfollowed by concentration under reduced pressure and purification of the product on a column of silica gel with ethyl acetatle-isopropyl alcohol (2.1) as eluant