反应详情

To a solution of ethyl nipecotate (20.0 mL, 130 mmol) in acetone (180 mL) was added 1-bromo-2-chloroethane (21.6 mL, 260 mmol) followed by anhydrous K2CO3 (27.12 g, 196 mmol). The reaction mixture was stirred for 24 h and then concentrated under vacuum. The resulting residue was treated with H2O (75 mL) and extracted with Et2O. The combined organic layers were dried with MgSO4, filtered, and concentrated under vacuum. Purification of the crude residue by flash chromatography (50% Et2O/50% hexane) on silica gel gave the title compound (10.99 g, 38.6%). EI-MS m/z 220(M+H+) Rt (1.20 min).

1. concentrationconcentrated under vacuum
2. additionThe resulting residue was treated with H2O (75 mL)
3. extractionextracted with Et2O
4. dry with materialThe combined organic layers were dried with MgSO4
5. filtrationfiltered
6. concentrationconcentrated under vacuum
7. customPurification of the crude residue by flash chromatography (50% Et2O/50% hexane) on silica gel