反应详情

To a 25 ml one necked round bottom flask 2-cyano-3-(4-(7-pivaloyl-5-((2-(trimethylsilyl)ethoxy)methyl)-5H-pyrrolo[2,3-b]pyrazin-2-ylamino)phenyl)acrylamide (0.1 g, 0.0002 mole) was taken in CH2Cl2 (10 ml). To this reaction mixture TFA (2.0 ml) was added dropwise at 0° C. After completion of the addition, the reaction mixture was warmed up to RT and then stirred for 16 hr. After completion of the reaction, CH2Cl2 was distilled out and the pH was adjusted to 8 to 9 using saturated NaHCO3 solution at 5° C. The reaction mixture was stirred for 15 min, solid was filtered, washed with n-pentane and dried. In a 25 ml RBF, dried solid was taken in ethanol and NaOAc. 3H2O (0.27 g, 0.002 mole) was added at RT. The reaction mixture was stirred for 20 hr at RT, diluted with ethyl acetate and distilled out under vacuum. To the resultant residual solid water was added, the mixture was stirred for 15 min, filtered, wash with water and n-pentane was added. The product was filtered and dried under vacuum to yield 20 mg of 2-cyano-3-(4-(7-pivaloyl-5H-pyrrolo[2,3-b]pyrazin-2-ylamino)phenyl)acrylamide.

1. additionAfter completion of the addition
2. distillationwas distilled out
3. customwas adjusted to 8 to 9 using saturated NaHCO3 solution at 5° C
4. stirringThe reaction mixture was stirred for 15 min
5. filtrationsolid was filtered
6. washwashed with n-pentane
7. customdried
8. customIn a 25 ml RBF, dried solid
9. addition3H2O (0.27 g, 0.002 mole) was added at RT
10. stirringThe reaction mixture was stirred for 20 hr at RT
11. additiondiluted with ethyl acetate
12. distillationdistilled out under vacuum
13. additionTo the resultant residual solid water was added
14. stirringthe mixture was stirred for 15 min
15. filtrationfiltered
16. washwash with water and n-pentane
17. additionwas added
18. filtrationThe product was filtered
19. customdried under vacuum