反应详情

To a solution of 5-[2-(6-methyl-pyridin-2-yl)-7H-pyrrolo[2,3-d]pyrimidin-4-yl]-nicotinic acid (Intermediate 5) (1 eq, 0.143 mmol, 50 mg) in MeCN (3 ml), ethylamine (1 eq, 0.143 mmol, 6.6 mg), EDC hydrochloride (1.5 eq, 0.215 mmol, 42 mg), HOBt (1.2 eq, 0.172 mmol, 23 mg), and TEA (5 eq, 0.720 mmol, 0.1 ml) are added. The mixture is heated using microwave radiation at 140° C. for 20 min. The resulting precipitate is filtered off and washed with MeCN. Drying the solid in vacuum affords the title compound; [M+H]+=359; 1H-NMR (400 MHz, CD3OD): δ 9.55 (d, 1H), 9.15 (t, 1H), 9.12 (d, 1H), 8.47 (d, 1H), 7.86 (t, 1H), 7.67 (d, 1H), 7.36 (d, 1H), 6.99 (d, 1H), 3.50 (q, 2H), 2.68 (s, 3H), 1.29 (t, 3H).

1. temperatureThe mixture is heated
2. customat 140° C.
3. customfor 20 min
4. filtrationThe resulting precipitate is filtered off
5. washwashed with MeCN
6. customDrying the solid in vacuum