HRID26026
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 5.0 g (15.2 mmol) of 1-(2,6-diethyl-4-nitrophenyl)-3-methylamidinourea hydrochloride and 5% paladium on carbon (500 mg) in absolute ethanol (175 ml) containing concentrated hydrochloric acid (2 ml) is shaken under an atmosphere of hydrogen (50 psi) for thirty minutes. The mixture is filtered through a Celite pad. To the filtrate is added HCl/MeOH and the alcohol is removed under vacuum to give a yellow foam which is crystallized from methanol-ethyl acetate to give 1-(4-amino-2,6-diethylphenyl)-3-methylamidinourea dihydrochloride, m.p. 218°-222° C. (dec).
WORKUP
后处理
- filtrationThe mixture is filtered through a Celite pad
- additionTo the filtrate is added HCl/MeOH
- customthe alcohol is removed under vacuum
- customto give a yellow foam which
- customis crystallized from methanol-ethyl acetate