反应详情

1-(4-Chlorophenyl)-N-[2-(4-methoxyphenyl)ethyl]cyclobutanecarboxamide (10.58 g, 30.8 mmol) was treated with toluene (100 mL). Phosphoryl trichloride (4.72 g, 30.8 mmol) was added and the reaction mixture was heated under reflux for 8 h. After cooling to room temperature the reaction mixture was concentrated in vacuo and then slowly poured in ice water. Ethyl acetate was added and the organic layer was washed with water (2×), dried (MgSO4) and concentrated in vacuo to give an orange oil. Yield: 10.25 g.

1. temperaturethe reaction mixture was heated
2. temperatureunder reflux for 8 h
3. concentrationwas concentrated in vacuo
4. additionslowly poured in ice water
5. additionEthyl acetate was added
6. washthe organic layer was washed with water (2×)
7. dry with materialdried (MgSO4)
8. concentrationconcentrated in vacuo
9. customto give an orange oil