反应详情

2-(6-Fluoro-1-methyl-1H-indazol-3-yl)-5-(2-trimethylsilanyl-ethoxymethyl)-5H-pyrrolo[2,3-b]pyrazine-7-carboxylic acid ((R)-1-methyl-2-pyrazol-1-yl-ethyl)-amide (86 mg, 0.16 mmol) was dissolved in dichloromethane (2.2 ml) and cooled in ice bath. Trifluoroacetic acid (1 ml) was slowly added and the reaction was stirred at room temperature for 2 h. The reaction was evaporated and the residue was dissolved in dichloromethane (1 ml). Ethylenediamine (0.63 ml, 9.4 mmol) was added and the mixture was stirred for 18 h. Water and then ethyl acetate were added to the mixture. The resulting precipitate was filtered off, rinsed with water and diethyl ether and dried under high vacuum to give 37 mg (57%) of 2-(6-fluoro-1-methyl-1H-indazol-3-yl)-5H-pyrrolo[2,3-b]pyrazine-7-carboxylic acid ((R)-1-methyl-2-pyrazol-1-yl-ethyl)-amide. MS: (M+Na)+=441; mp=252-253° C. 1H NMR (300 MHz, DMSO-d6) δ: 9.08 (s, 1H), 8.46 (s, 1H), 8.21-8.33 (m, 1H), 8.12 (d, J=7.9 Hz, 1H), 7.63-7.75 (m, 2H), 7.31-7.40 (m, 1H), 6.97-7.10 (m, 1H), 6.12-6.23 (m, 1H), 4.46-4.63 (m, 1H), 4.32-4.44 (m, 2H), 4.14 (s, 3H), 1.23 (d, J=6.4 Hz, 3H).

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