反应详情

The diethyl 2-((thiophen-3-ylamino)methylene)malonate 2 (1.0 g, 3.7 mmol, 1 eq) was heated to 240° C. in Ph2O (10 mL) for 6 h. After the starting material was consumed, the reaction mixture was allowed to cool to room temperature and solid was filtered. The solid was washed with water and dichloromethane to obtain the desired compound as a light brown powder (0.42 g 50% yield). LC/MS (10-99% CH3CN/0.05% TFA gradient over 5 min): m/z 224.0, retention time 0.40 minutes. 1H NMR (DMSO-d6) δ: 12.80 (s, 1.0H), 8.50 (s, 1.0H), 8.05 (d, 1.0H, J=5.4 Hz), 7.30 (d, 1.0H, J=5.4 Hz), 4.20 (q, 2H, J=7.0 Hz), 4.10 (q, 2H, J=7.0 Hz), 1.30 (t, 3H, J=7.0 Hz).

1. customAfter the starting material was consumed
2. filtrationsolid was filtered
3. washThe solid was washed with water and dichloromethane