反应详情

To a solution of 6-benzyloctahydro-1H-pyrrolo[3,4-b]pyridine (5.00 g) in THF was added 80% NaH (3.00 g) at room temperature. The reaction mixture was stirred for 30 min, and 5.3 mL of iodoethane was added dropwise. The reaction mixture was stirred for another 5 h, and then quenched with ice-water. The resulted mixture was extracted with CH2Cl2 (70 mL×5). The combined organic phases were dried over anhydrous Na2SO4 and concentrated in vacuo. The residue was chromatographed with a silica gel column (eluting agent: 30:1 (v/v) DCM/MeOH) to give the title compound as a pale yellow solid (2.58 g, 45.60%). The compound was characterized by the following spectroscopic data: MS (ESI, pos. ion) m/z: 245.2 (M+1).

1. stirringThe reaction mixture was stirred for another 5 h
2. customquenched with ice-water
3. extractionThe resulted mixture was extracted with CH2Cl2 (70 mL×5)
4. dry with materialThe combined organic phases were dried over anhydrous Na2SO4
5. concentrationconcentrated in vacuo
6. customThe residue was chromatographed with a silica gel column (eluting agent: 30:1 (v/v) DCM/MeOH)