反应详情

To a stirred solution of 4-[6-(2-ethoxy-phenyl)-pyrimidin-4-ylcarbamoyl]-piperidine-1-carboxylic acid tert-butyl ester (IV), (0.500 g, 1.17 mmol) in dry dichloromethane (1.5 ml), TFA (1.5 ml) was added at 0° C. and the reaction mixture was stirred for 2-3 hours. After completion of the reaction (monitored by TLC) the solvent mixture was removed under reduced pressure and dichloromethane was added to the residue. Solid sodium carbonate was added and the mixture was stirred for 3-4 hours. Then it was filtered and washed with dichloromethane. The combined filtrate was concentrated under reduced pressure to obtain a solid which was washed with 10% ethyl acetate/hexane to remove nonpolar impurities, giving piperidine-4-carboxylic acid [6-(2-ethoxy-phenyl)-pyrimidin-4-yl]-amide (compound #1A) as pure white solid (0.19 g, 50%).

1. customAfter completion of the reaction (monitored by TLC) the solvent mixture
2. customwas removed under reduced pressure and dichloromethane
3. additionwas added to the residue
4. additionSolid sodium carbonate was added
5. stirringthe mixture was stirred for 3-4 hours
6. filtrationThen it was filtered
7. washwashed with dichloromethane
8. concentrationThe combined filtrate was concentrated under reduced pressure
9. customto obtain a solid which
10. washwas washed with 10% ethyl acetate/hexane
11. customto remove nonpolar impurities