HRID442250
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
The dioxime from Step 2 (30 g) is dissolved in ethyl alcohol (300 ml), saturated with ammonia gas and Raney nickel catalyst W-6 (2 g) added. The mixture is subjected to 700 psi hydrogen pressure and heated at 70° for 3 hours. The catalyst is removed by filtration and 220 ml of ethanol is removed by distillation. The pale yellow precipitate is filtered and dried. Yield 28 g (91% of theory) mp 123°-127°. Calculated for C20H20N2 : C, 83.29%; H, 6.99%; N, 9.71%. Found: C, 83.07%; H, 6.89%; N, 9.59%.
WORKUP
后处理
- addition(2 g) added
- temperatureheated at 70° for 3 hours
- customThe catalyst is removed by filtration and 220 ml of ethanol
- customis removed by distillation
- filtrationThe pale yellow precipitate is filtered
- customdried