反应详情

300 mg (0.76 mmol) of 3-(3-amino-4-trifluoromethoxyphenyl)5,5-dimethyl-1-pyridin-4-ylmethylimidazolidine-2,4-dione were dissolved in 15 ml of ethyl acetate, admixed with 492 mg (1.52 mmol) of 1-cyclohexylazetidin-3-yl methanesulphonate oxalate and 631 mg (4.56 mmol) of K2CO3, and heated under reflux for 4 h. To complete the reaction, a further 49 mg (0.15 mmol) of 1-cyclohexylazetidin-3-yl methanesulphonate oxalate and 63 mg (0.46 mmol) of K2CO3 were added, and the mixture was stirred under reflux once again for 2 h. Subsequently, the mixture was concentrated and the residue purified by flash chromatography (150 g of silica gel/95:5 CH2C12:CH3OH).

1. temperatureheated
2. temperatureunder reflux for 4 h
3. customthe reaction
4. temperatureunder reflux once again for 2 h
5. concentrationSubsequently, the mixture was concentrated
6. customthe residue purified by flash chromatography (150 g of silica gel/95:5 CH2C12:CH3OH)