反应详情

To a solution of N-tert-butyl-2-(5-(methylsulfonyl)pyridin-3-ylamino)-5-((2-(trimethylsilyl)ethoxy)methyl)-5H-pyrrolo[2,3-b]pyrazine-7-carboxamide (125 mg, 241 mol) in dichloromethane was added trifluoroacetic acid (550 mg, 371 μL, 4.82 mmol) and the mixture stirred at room temperature for 16 h. The mixture was concentrated then re-dissolved in dichloromethane (3.7 mL), methanol (1.6 mL) and ammonium hydroxide (0.5 mL) and the mixture stirred at room temperature for 1 h. The mixture was concentrated in vacuo then triturated with water and filtered. The solid obtained was washed with ether then dried to give N-tert-butyl-2-(5-(methylsulfonyl)pyridin-3-ylamino)-5H-pyrrolo[2,3-b]pyrazine-7-carboxamide (92 mg, 237 mol, 98%) as a yellow solid. 1H NMR (400 MHz, DMSO-d) δ ppm: 12.38 (s, 1H), 9.90 (s, 1H), 9.40 (d, J=2.5, 1 H), 8.55 (d, J=1.9, 1 H), 8.06 (t, J=2.2, 1H), 8.01 (s, 1H), 7.96 (s, 1H), 7.54 (s, 1H), 3.22 (s, 3H), 1.31 (s, 9H); MS (EI/CI) m/z: 389.1 [M+H].

1. concentrationThe mixture was concentrated
2. dissolutionthen re-dissolved in dichloromethane (3.7 mL)
3. stirringmethanol (1.6 mL) and ammonium hydroxide (0.5 mL) and the mixture stirred at room temperature for 1 h
4. concentrationThe mixture was concentrated in vacuo
5. customthen triturated with water
6. filtrationfiltered
7. customThe solid obtained
8. washwas washed with ether
9. customthen dried