反应详情

To a cooled (0° C.) suspension of 2,4-dichloropyrimidine (20)(1.0 g, 6.7 mmol) in ethanol (20 ml), which was stirred under an inert atmosphere, was added triethylamine (1.4 ml, 10.1 mmol) and then morpholine (0.59 ml, 6.7 mmol). The mixture was maintained at this temperature for 3 hours whereupon it was concentrated in vacuo, diluted with NaOH (20 ml, 1M) and extracted with EtOAc (3×20 ml). The organic extracts were combined, dried (Na2SO4), filtered and concentrated in vacuo to give a colorless solid. The crude residue was re-crystallised using EtOAc/Hexanes to give the title compound (1.21 g, 90%) as a colourless solid which required no further purification. m/z (LC-MS, ESP): 200 [M+H]+, R/T=3.26 mins

1. temperatureTo a cooled
2. temperatureThe mixture was maintained at this temperature for 3 hours whereupon it
3. concentrationwas concentrated in vacuo
4. additiondiluted with NaOH (20 ml, 1M)
5. extractionextracted with EtOAc (3×20 ml)
6. dry with materialdried (Na2SO4)
7. filtrationfiltered
8. concentrationconcentrated in vacuo
9. customto give a colorless solid
10. customThe crude residue was re-crystallised