HRID359461
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
To 8-amino-5,6,7,8-tetrahydro-3-methylquinoline (4.5g, 2.27 M moles) in CH2Cl2 was added 4-nitrobenzoylchloride (4.2g, 2.26Mmoles) followed by sufficient triethylamine to clear the solution and then form a new precipitate. This material was left overnight and then the solvent removed. The residue was taken up in 2M HCl and washed with ethyl acetate. The aquous layer was then basified with Na2CO3 and extracted with chloroform. The organic solution was dried (MgSO4) and evaporated under reduced pressure to give a residue which was treated with Et2O/HCl to give a white solid identified by infra-red and nmr specroscopy as the hydrochloride of the title compound.
WORKUP
后处理
- customform a new precipitate
- customthe solvent removed
- washwashed with ethyl acetate
- extractionextracted with chloroform
- dry with materialThe organic solution was dried (MgSO4)
- customevaporated under reduced pressure
- customto give a residue which
- customto give a white solid