反应详情

A mixture of 4-chlorocarbonyl-piperidine-1-carboxylic acid benzyl ester (VII) (5.70 g, 20.2 mmol), 4-amino-6-chloropyrimidine (I) (2.10 g, 16.2 mmol) and 4-(N,N-dimethylamino)-pyridine (2.90 g, 23.7 mmol) in dichloromethane (50 ml) was heated to reflux temperature for 18 hours. The progress of the reaction was monitored by TLC, then dichloromethane was completely distilled off. Aqueous sodium bicarbonate solution was added to the residue and the mixture was extracted with ethyl acetate (3×100 ml). The organic layers were separated, dried over sodium sulfate and concentrated to obtain 4-(6-chloro-pyrimidin-4-ylcarbamoyl)-piperidine-1-carboxylic acid benzyl ester (VIII) (5.9 g, 79%) as a yellow solid.

1. temperaturewas heated
2. temperatureto reflux temperature for 18 hours
3. distillationdichloromethane was completely distilled off
4. additionAqueous sodium bicarbonate solution was added to the residue
5. extractionthe mixture was extracted with ethyl acetate (3×100 ml)
6. customThe organic layers were separated
7. dry with materialdried over sodium sulfate
8. concentrationconcentrated