反应详情

1,3-Cyclohexanediol (116 mg, 1.0 mmole) was added to a flame dried round bottom flask under nitrogen. The flask was then charged with 5 mL of dry acetonitrile, 26 mg of potassium fluoride on alumina (0.1 mmol), and 4-fluoro-2-chloro-benzonitrile (155 mg, 1.0 mmole) and heated at reflux for 16 h. Diethyl ether (15 ml) was added to the reaction mixture, which was then extracted with water (2×), dried (MgSO4) and concentrated. Purification using a chromatotron, eluting with 10% EtOAc/hex (ethylacetate and hexane) provided 22 mg of the title compound. GC/MS: 251 (M/Z for C13H14ClNO2).

1. customdried round bottom flask under nitrogen
2. temperatureheated
3. temperatureat reflux for 16 h
4. extractionwas then extracted with water (2×)
5. dry with materialdried (MgSO4)
6. concentrationconcentrated
7. customPurification
8. washeluting with 10% EtOAc/hex (ethylacetate and hexane)