反应详情

温度

90 °C

A mixture of 2,6-dichloro-4-aminopyrimidine 6-1 (4.8 g, 29.3 mmol), ethylamine hydrochloride (7.0 g, 85.8 mmol), Et3N (20 mL, 144 mmol) and n-butanol (150 mL) was heated to 90° C. for 6 hours. After cooling, the solvent was removed in vacuo and the residue partitioned between saturated Na2CO3 solution and EtOAc. The EtOAc layer was washed with brine, dried (MgSO4) and concentrated to give an orange solid. Purification by column chromatography (EtOAc/hexane 1:1) gave the title compound 6-2 as a white solid.

1. temperatureAfter cooling
2. customthe solvent was removed in vacuo
3. customthe residue partitioned between saturated Na2CO3 solution and EtOAc
4. washThe EtOAc layer was washed with brine
5. dry with materialdried (MgSO4)
6. concentrationconcentrated
7. customto give an orange solid
8. customPurification by column chromatography (EtOAc/hexane 1:1)