반응 #545059

반응 방정식

4-(3-fluorophenyl)-5-(2-fluoro-4-pyridyl)-2-pyrimidinylamine

ammonia ethanol

ammonia

→

title compound

수율 12.0%

5-(2-Amino-4-pyridyl)-4-(3-fluorophenyl)-2-pyrimidinylamine

수율 12.0%

용매

ethanol

반응 조건

후처리

1. 1
   온도cooling) (20 mL)
2. 2
   기타was sealed in a test tube
3. 3
   온도After cooling as it
4. 4
   농축the reaction solution was concentrated
5. 5
   workup.DISSOLUTIONThe residue was dissolved
6. 6
   workup.ADDITIONby adding ethyl acetate and water
7. 7
   세척The organic layer was washed with water and brine
8. 8
   건조dried over anhydrous sodium sulfate
9. 9
   농축concentrated
10. 10
    기타The residue was purified by TLC plate (eluting solvent: dichloromethane/methanol=10/1)

실험 절차

A mixture of 4-(3-fluorophenyl)-5-(2-fluoro-4-pyridyl)-2-pyrimidinylamine (100 mg, 0.352 mmol) and ammonia/ethanol (ethanol saturated with an ammonia gas under ice-cooling) (20 mL) was sealed in a test tube and stirred at 150° C. for 2 weeks. After cooling as it was, the reaction solution was concentrated. The residue was dissolved by adding ethyl acetate and water thereto. The organic layer was washed with water and brine, and then dried over anhydrous sodium sulfate and concentrated. The residue was purified by TLC plate (eluting solvent: dichloromethane/methanol=10/1), to give the title compound (12 mg, 12%).

출처