反应详情

温度

200 °C

To a stirred solution of the product of step (a) (500 mg) and 4,4,5,5,5-pentafluoropentan-1-ol (284 mg) in tetrahydrofuran (10 ml) was added potassium tert-butoxide (1M in tetrahydrofuran; 1.6 ml) and the reaction was stirred at 200° C. for 2 hours. An additional charge of potassium tert-butoxide (1M in tetrahydrofuran; 1.6 ml) was added and the reaction was stirred for a further 18 hours. Ethanol (5 ml) was added and the reaction was stirred for 30 mlnutes. The reaction mixture was partitioned between dichloromethane (300 ml) and water (300 ml). The organic layer was dried over magnesium sulphate and the solvent was removed in vacuo. Purification by column chromatography on silica gel (5 g Bond Elut cartridge) eluting with 20% ethyl acetate in cyclohexane gave the title compound as a clear oil (100 mg).

1. additionwas added
2. stirringthe reaction was stirred for a further 18 hours
3. stirringthe reaction was stirred for 30 mlnutes
4. customThe reaction mixture was partitioned between dichloromethane (300 ml) and water (300 ml)
5. dry with materialThe organic layer was dried over magnesium sulphate
6. customthe solvent was removed in vacuo
7. customPurification by column chromatography on silica gel (5 g Bond Elut cartridge)
8. washeluting with 20% ethyl acetate in cyclohexane