HRID2299696
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
Under nitrogen, a solution of 3-oxiranylpyridine (1.9 g) and N-benzyl-(3-methoxy-6,7,8,9-tetrahydro-5H-benzocyclohepten-6-yl)amine (3.3 9) in ethanol (15 ml) was refluxed for 5 hours. After removal of ethanol in vacuo, the residue was dissolved into a mixture of aqueous sodium hydrogencarbonate and ethyl acetate. After separation, the organic layer was washed with brine, dried over anhydrous magnesium sulfate and evaporated in vacuo. The residue was purified by column chromatography on silica gel (chloroform:methanol=20:1) to give 2-[N-benzyl-N-(3-methoxy-6,7,8,9-tetrahydro-5H-benzocyclohepten-6-yl) amino]-1-(pyridin-3-yl)ethanol (520 mg).
WORKUP
后处理
- customAfter removal of ethanol in vacuo
- dissolutionthe residue was dissolved into a mixture of aqueous sodium hydrogencarbonate and ethyl acetate
- customAfter separation
- washthe organic layer was washed with brine
- dry with materialdried over anhydrous magnesium sulfate
- customevaporated in vacuo
- customThe residue was purified by column chromatography on silica gel (chloroform:methanol=20:1)