HRID860180
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
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
- temperatureThe reaction mixture was refluxed for 5 minutes after which it
- filtrationthe residue filtered off
- temperatureunder reflux for 5 h
- customafter which the solvent was removed under vacuum
- customto give a white solid