HRID1907441
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
CONDITIONS
反应条件
- 温度
- 80 °C
PROCEDURE
实验过程
To a solution of 1-methyl-4-(4-methyl-3-nitro-phenyl)-piperazine (9.0 g, 38.29 mmol) in ethanol (100 mL) and cyclohexene (7 ml), Pd/C 10% (1.5 g) was added. The mixture was heated at 80° C. for 6 hours until HPLC revealed the disappearance of the starting material. The Pd was filtered from the reaction and the solvents were removed from the filtrate under reduced pressure. The crude was diluted with DCM and treated with HCl in dioxane; the precipitate was collected and washed with diethyl ether to give the final compound as a brown solid in quantitative yield.
WORKUP
后处理
- filtrationThe Pd was filtered from the reaction
- customthe solvents were removed from the filtrate under reduced pressure
- additionThe crude was diluted with DCM
- additiontreated with HCl in dioxane
- customthe precipitate was collected
- washwashed with diethyl ether