[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][CH:12]=1)[C:9](=O)[CH2:8][CH2:7][CH2:6]2.[C-]#N.[K+].[C:17](=[O:20])([O-])[O-].[NH4+:21].[NH4+:22].C[CH2:24][OH:25]>O>[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][CH:12]=1)[C:9]1([C:24](=[O:25])[NH:22][C:17](=[O:20])[NH:21]1)[CH2:8][CH2:7][CH2:6]2A mixture of 35.2 g (0.2 mol) of 6-methoxy-1-tetralone, 19.5 g (0.3 mol) of potassium cyanide and 134.4 g (1.4 mol) of ammonium carbonate in 280 mL of EtOH was placed in a stainless steel bomb and heated at 110° C. for 48 hours. After cooling, the mixture was poured in 1.4 L of water. It was allowed to sit at ambient temperature for 3 days. The precipitated solid was filtered and washed several times with water and dried to give 48.1 g of a brown solid: mp 218°-220° C. 1H-NMR (DMSO-d6)d10.75(s, 1H),8.45(s, 1H),6.96(d, 1H),6.79 (d, 1H), 6.70 (s, 1H), 3.72 (s, 3H), 2.73 (t, 2H), 1.70-2.20 (m, 4H).
読み込み中…
