HRID1679923
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
20.4 g (88.2 millimoles) of 2-(m-nitrophenyl)-3,4-diaza-bicyclo[4.1.0]hept-2-en-5-one (see Example 32b), 300 ml of ethanol, 150 ml of cyclohexene and 4.2 g of 10% strength palladium on charcoal are refluxed for 12 hours. The catalyst is filtered off, the filtrate is concentrated and the residue is recrystallized from ethyl acetate/methanol. 8.5 g (48% of theory) of 2-(m-aminophenyl)-3,4-diaza-bicyclo[4.1.0]hept-2-en-5-one are obtained as beige crystals, of melting point 192°-193° C.
WORKUP
后处理
- filtrationThe catalyst is filtered off
- concentrationthe filtrate is concentrated
- customthe residue is recrystallized from ethyl acetate/methanol