反应详情

To a solution of tert-butyl octahydro-1H-pyrrolo[3,2-c]pyridine-1-carboxylate (0.63 g) in acetone (15 mL) was added K2CO3 (1.54 g) and 1-bromo-3-chloropropane (1.45 mL). The reaction mixture was heated to reflux overnight, diluted with water and extracted with EtOAc. The organic layer was dried over anhydrous Na2SO4 for 1 h and filtered. The filtrate was concentrated in vacuo and the residue was chromatographed with a silica gel column (eluting agent: 10:1 (v/v) CH2Cl2/MeOH) to give the title compound as pale yellow liquid (0.65 g, 77.00%).

1. temperatureThe reaction mixture was heated
2. temperatureto reflux overnight
3. extractionextracted with EtOAc
4. dry with materialThe organic layer was dried over anhydrous Na2SO4 for 1 h
5. filtrationfiltered
6. concentrationThe filtrate was concentrated in vacuo
7. customthe residue was chromatographed with a silica gel column (eluting agent: 10:1 (v/v) CH2Cl2/MeOH)