反应详情

To a room temperature solution of piperidine (284 mg, 3.33 mmol) in CH2Cl2 (5 mL) was added trimethylaluminum (2M in hexane, 1.7 mL, 3.4 mmol). After 15 min, the product from Step 1 (310 mg, 0.92 mmol) was added in one portion and the mixture was heated to reflux for 20 h. The resulting solution was cooled and poured into 1M HCl (gas evolution). The organic layer was washed with brine, filtered through cotton and evaporated. Purification by flash chromatography (80% EtOAc/Hex) provided 175 mg of the title compound.

1. temperaturethe mixture was heated
2. temperatureto reflux for 20 h
3. temperatureThe resulting solution was cooled
4. washThe organic layer was washed with brine
5. filtrationfiltered through cotton
6. customevaporated
7. customPurification by flash chromatography (80% EtOAc/Hex)