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
4-Amino-6,7-dimethoxy-2-(4-benzylpiperazin-1-yl)quinoline (6.2 g) in ethanol (300 ml) with 5% Pd/C catalyst was stirred at 50° under an atmosphere of hydrogen (50 p.s.i.) for 20 hours. The mixture was cooled, chloroform (100 ml) added and the solution filtered through "Solkafloc". The solid was washed with chloroform-methanol (1:1, 4×100 ml) and the combined filtrates evaporated in vacuo. The residue was partitioned between chloroform-sodium carbonate solution (10%), the organic layer removed, the aqueous phase saturated with salt and further extracted with chloroform. The combined organic extracts were washed with brine, dried (Na2SO4) and evaporated in vacuo to yield 4-amino-6,7-dimethoxy-2-(piperazin-1-yl)quinoline (2.42 g). Spectroscopy showed this product to be the same as that of Example 32.
WORKUP
后处理
- temperatureThe mixture was cooled
- filtrationthe solution filtered through "Solkafloc"
- washThe solid was washed with chloroform-methanol (1:1, 4×100 ml)
- customthe combined filtrates evaporated in vacuo
- customThe residue was partitioned between chloroform-sodium carbonate solution (10%)
- customthe organic layer removed
- extractionthe aqueous phase saturated with salt and further extracted with chloroform
- washThe combined organic extracts were washed with brine
- dry with materialdried (Na2SO4)
- customevaporated in vacuo