반응 #58708

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mixture

Ethyl 3-[(2-cyanophenyl)amino]-6-oxo-7-(3-thienyl)-6,7-dihydrothieno[2,3-b]pyridine-2-carboxylate

2-ethoxyethanol

ammonia

→

title compound

3-[(2-Cyanophenyl)amino]-6-oxo-7-(3-thienyl)-6,7-dihydrothieno[2,3-b]pyridine-2-carboxamide

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후처리

1. 1
   기타The volatiles were removed in vacuo
2. 2
   기타the residue purified by column chromatography (silica, EtOAc)

실험 절차

A mixture of Example 66 (100 mg), 2-ethoxyethanol and liquid ammonia was placed in a sealed pressure vessel and heated at 80° C. and 400 psi for 48 h. The volatiles were removed in vacuo and the residue purified by column chromatography (silica, EtOAc) to give the title compound (30 mg). δH (CDCl3) 7.59-7.46 (4H, m), 7.28-7.21 (3H, m), 7.20 (1H, t, J 2.0 Hz), 7.01 (1H, d, J 8.3 Hz), 6.49 (1H, d, J 9.7 Hz), 5.55 (2H, br s). LCMS (ES+) RT 2.845 minutes, 392.9 (M+H)+

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