反应详情

2-(6-Chloro-1-methyl-1H-indazol-3-yl)-5-(2-trimethylsilanyl-ethoxymethyl)-5H-pyrrolo[2,3-b]pyrazine-7-carboxylic acid isopropylamide (45 mg, 0.09 mmol) was dissolved in dichloromethane (0.9 ml) and cooled in ice bath. Trifluoroacetic acid (0.3 ml) was added slowly and the reaction was stirred at room temperature for 3.5 h. The reaction was evaporated and the residue was dissolved in dichloromethane (2 ml). Ethylenediamine (0.36 ml, 5.4 mmol) was added and the mixture was stirred at room temperature for 18 h. Water and then ethyl acetate were added to the mixture. The resulting precipitate was filtered off, rinsed with water and dried under high vacuum to give 21 mg (81%) of 2-(6-chloro-1-methyl-1H-indazol-3-yl)-5H-pyrrolo[2,3-b]pyrazine-7-carboxylic acid isopropylamide. (M+Na)+=391; mp=356-362° C. 1H NMR (400 MHz, DMSO-d6) δ ppm 12.79-12.90 (m, 1H) 9.09 (s, 1H) 8.44 (d, J=9.1 Hz, 1H) 8.42 (s, 1H) 8.02 (d, J=7.6 Hz, 1H) 8.00 (d, J=1.5 Hz, 1H) 7.30 (dd, J=8.8, 1.8 Hz, 1H) 4.19-4.27 (m, 1H) 4.17 (s, 3H) 1.32 (d, J=6.6 Hz, 6H).

1. temperaturecooled in ice bath
2. customThe reaction was evaporated
3. dissolutionthe residue was dissolved in dichloromethane (2 ml)
4. stirringthe mixture was stirred at room temperature for 18 h
5. filtrationThe resulting precipitate was filtered off
6. washrinsed with water
7. customdried under high vacuum