反应详情

In a 10 ml round-bottomed flask, 2-(1-methyl-1H-pyrazolo[4,3-b]pyridin-3-yl)-5-(2-trimethylsilanyl-ethoxymethyl)-5H-pyrrolo[2,3-b]pyrazine-7-carboxylic acid tert-butylamide (49 mg, 0.102 mmol) was dissolved in dichloromethane (0.6 ml) and trifluoroacetic acid (0.32 ml, 4.15 mmol) was added. The yellow reaction mixture was stirred at room temperature for 2 h then concentrated. The residue was dissolved in dichloromethane (0.6 ml) and ethylenediamine (0.42 ml, 6.22 mmol) was added. The yellow solution was stirred at room temperature for 1 h then quenched with water and diluted with ethyl acetate. The resulting suspension was filtered and washed with hot water and ethyl acetate and the product dried under high vacuum to provide 23 mg (64%) of 2-(1-methyl-1H-pyrazolo[4,3-b]pyridin-3-yl)-5H-pyrrolo[2,3-b]pyrazine-7-carboxylic acid tert-butylamide as a light yellow powder. MS: (M+H)+=350; 1H NMR (DMSO-d6, 400 MHz): δ (ppm) 12.58 (br. s., 1H), 9.34 (s, 1H), 8.69 (s, 1H), 8.65 (dd, J=4.3, 1.3 Hz, 1H), 8.34 (s, 1H), 8.27 (dd, J=8.6, 1.3 Hz, 1H), 7.52 (dd, J=8.6, 4.3 Hz, 1H), 4.21 (s, 3H), 1.53 (s, 9H).

1. concentrationthen concentrated
2. dissolutionThe residue was dissolved in dichloromethane (0.6 ml)
3. stirringThe yellow solution was stirred at room temperature for 1 h
4. customthen quenched with water
5. additiondiluted with ethyl acetate
6. filtrationThe resulting suspension was filtered
7. washwashed with hot water and ethyl acetate
8. customthe product dried under high vacuum