反应详情

To 1,2,3,4-tetrahydro-isoquinoline (9.4 mmol) in DMF (10 ml), 3-bromo-propyne (4.5 mmol) is added at 0° C. and stirred at room temperature for 18 h. After the reaction mixture is treated with saturated ammonium chloride, the mixture is extracted with AcOEt. The organic layer is washed with brine, dried over magnesium sulfate and evaporated down. The crude product is applied to a silica gel column chromatography, which is eluted with following solvents: n-hexane and n-hexane:AcOEt=1:1 (v/v). The solvent of the latter effluent is removed by evaporation and dried in vacuo to afford the title compound. yield 91.2%, Rf=0.67 (n-hexane:AcOEt=1:5).

1. extractionthe mixture is extracted with AcOEt
2. washThe organic layer is washed with brine
3. dry with materialdried over magnesium sulfate
4. customevaporated down
5. washis eluted with following solvents
6. customThe solvent of the latter effluent is removed by evaporation
7. customdried in vacuo