反应详情

Suspend 1.65 g (3.9 mmol) of (+/−)-({3-[(6-phenylfuro[2,3-d]pyrimidin-4-yl)amino]cyclohexyl}-oxy)acetic acid tert-butyl ester in 4 ml of carbon tetrachloride and add 762 mg (4.3 mmol) of N-bromosuccinimide. Heat the reaction mixture under reflux for 1 h. After cooling to RT, add a further 350 mg of N-bromosuccinimide. Stir the reaction mixture under reflux again for 1 h, then cool and concentrate under reduced pressure. From the residue, after purification by chromatography on silica gel (eluent: cyclohexane/ethyl acetate 5:1), 0.99 g of the target product is isolated (50.6% of theory).

1. temperatureHeat the reaction mixture
2. temperatureunder reflux for 1 h
3. temperatureunder reflux again for 1 h
4. temperaturecool
5. concentrationconcentrate under reduced pressure
6. customFrom the residue, after purification by chromatography on silica gel (eluent: cyclohexane/ethyl acetate 5:1)