反应详情

温度

105 °C

2,3-Diamino-4,5-dichloropyridine (Example 206a) (0.10 g, 0.56 mmol) and 4-morpholin-4-ylbenzoic acid (0.12 g, 0.56 mmol) were dissolved in POCl3 (5 ml) and heated to 105° C. for 5 h. The excess of POCl3 was evaporated off and the residue was dissolved in EtOAc and aqueous K2CO3. The aqueous phase was extracted three times with EtOAc. The combined organic phases were washed with brine, dried (Na2SO4), evaporated in vacuo and the residue was purified by HPLC-C18. The product crystallized from the chromatography fraction and was filtered off and dried to yield a white powder (0.040 g, 20%).

1. customThe excess of POCl3 was evaporated off
2. dissolutionthe residue was dissolved in EtOAc
3. extractionThe aqueous phase was extracted three times with EtOAc
4. washThe combined organic phases were washed with brine
5. dry with materialdried (Na2SO4)
6. customevaporated in vacuo
7. customthe residue was purified by HPLC-C18
8. customThe product crystallized from the chromatography fraction
9. filtrationwas filtered off
10. customdried