反应详情

2-[6-Chloro-1-(2-dimethylamino-ethyl)-1H-indazol-3-yl]-5-(2-trimethylsilanylethoxymethyl)-5H-pyrrolo[2,3-b]pyrazine-7-carboxylic acid ((S)-2-methoxy-1-methyl-ethyl)amide (50 mg, 0.085 mmol) was combined with dichloromethane (1 mL) and trifluoroacetic acid (0.19 ml, 2.56 mmol) was added. After stirring for 2 h, the reaction mixture was concentrated in vacuo and the residue was dissolved in dichloromethane (1 mL). Ethylenediamine (0.17 ml, 2.56 mmol) was added. After stirring for 20 min, the reaction was concentrated in vacuo. The residue was triturated with water (2 mL). The precipitate was filtered, washed with water and dried to obtain 30 mg (73%) of 2-[6-chloro-1-(2-dimethylamino-ethyl)-1H-indazol-3-yl]-5H-pyrrolo[2,3-b]pyrazine-7-carboxylic acid ((S)-2-methoxy-1-methyl-ethyl)-amide as a yellow solid. MS: (M+H)+=456; 1H NMR (DMSO-d6) δ: 9.11 (s, 1H), 8.51 (d, J=8.5 Hz, 1H), 8.44 (s, 1H), 8.45 (s., 1H), 8.20 (d, J=8.0 Hz, 1H), 8.06 (s, 1H), 7.26 (d, J=8.3 Hz, 1H), 4.62 (br. s., 2H), 4.38 (br. s., 1H), 3.50 (dd, J=16.1, 4.0 Hz, 2H), 3.28 (s, 3H), 2.81 (br. s., 2H), 2.21 (s, 6H), 1.31 (d, J=6.5 Hz, 3H).

1. additionwas added
2. concentrationthe reaction mixture was concentrated in vacuo
3. dissolutionthe residue was dissolved in dichloromethane (1 mL)
4. stirringAfter stirring for 20 min
5. concentrationthe reaction was concentrated in vacuo
6. customThe residue was triturated with water (2 mL)
7. filtrationThe precipitate was filtered
8. washwashed with water
9. customdried