反应详情

温度

0 °C

Methyl 3-(cyclopentylamino)propanoate (838 mg, 0.005 mol) and K2CO3 (676 mg, 0.005 mol) were added to acetone (5 ml) and the resulting mixture cooled to 0° C. using an ice-bath before the addition of 2,4-dichloro-5-nitropyrimidine (1.044 g, 1.1 eq). The reaction mixture (RM) was then warmed to rt and stirring continued for an additional 16 h before the addition of a further 0.12 eq of the pyrimidine. Stirring was then continued for a further 3 h. The RM was then evaporated under reduced pressure and the product extracted using EtOAc/H2O. The organic extracts were combined, washed with sat NaCl, dried using MgSO4, filtered and the filtrate evaporated under reduced pressure and further dried in vacuo to give the product as a brown oily residue (1.04 g, 65%); Rt=16 min (Vydac 1); ME+ve: 329.1.

1. temperatureThe reaction mixture (RM) was then warmed to rt
2. stirringStirring
3. customThe RM was then evaporated under reduced pressure
4. extractionthe product extracted
5. washwashed with sat NaCl
6. customdried
7. filtrationfiltered
8. customthe filtrate evaporated under reduced pressure
9. customfurther dried in vacuo