反应详情

To a solution of 1-benzyl-4-chloro-5,5-dimethyl-1,2,5,6-tetrahydropyridine-3-carbaldehyde (75 g, 0.28 mol) in DCM (1.2 L) was added ethyl 2-mercaptoacetate (67 g, 0.56 mol) and triethylamine (85 g, 0.84 mol) was added slowly at room temperature. Upon complete addition, the reaction mixture was heated at reflux overnight. Upon cooling to room temperature, the reaction was quenched with the addition of water. The organic layer was washed with water, dried over anhydrous Na2SO4, concentrated and purified by silica gel chromatography (0-20% EtOAc/hexane) to afford the title compound (31.7 g, 27.5% over two steps).

1. additionwas added slowly at room temperature
2. additionUpon complete addition
3. temperaturethe reaction mixture was heated
4. temperatureat reflux overnight
5. customthe reaction was quenched with the addition of water
6. washThe organic layer was washed with water
7. dry with materialdried over anhydrous Na2SO4
8. concentrationconcentrated
9. custompurified by silica gel chromatography (0-20% EtOAc/hexane)