HRID860180

反应详情

EQUATION

反应方程式

HRID 860180 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

536 mg (5 mmol) benzylamine and 1.17 g (5 mmol) S′-methylthiosemicarbazide hydroiodide was mixed in 10 ml of ethanol. The reaction mixture was refluxed for 5 minutes after which it was cooled down to room temperature and the residue filtered off. The crude product of N-amino-N′-benzylguanidine was reacted with 1.0 g (5 mmol) 2-chloro-3,4-dimethoxybenzaldehyde under reflux for 5 h, after which the solvent was removed under vacuum to give a white solid. The product was obtained by recrystallisation from methanol. Yield of title compound 1, was 1.65 g (77%). M.p. 0.223–225° C.

WORKUP

后处理

  1. temperatureThe reaction mixture was refluxed for 5 minutes after which it
  2. filtrationthe residue filtered off
  3. temperatureunder reflux for 5 h
  4. customafter which the solvent was removed under vacuum
  5. customto give a white solid