Dimethylamine → HCID 19599959、化合物

反応式

[C:1]1([CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][N:13]2[CH2:19][CH2:18][CH2:17][C:16]3[CH:20]=[CH:21][O:22][C:15]=3[CH2:14]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH3:23][NH:24][CH3:25].[CH2:26]=O>C(O)(=O)C>[CH3:23][N:24]([CH2:26][C:21]1[O:22][C:15]2[CH2:14][N:13]([CH2:12][CH2:11][CH2:10][CH2:9][CH2:8][CH2:7][C:1]3[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=3)[CH2:19][CH2:18][CH2:17][C:16]=2[CH:20]=1)[CH3:25]

参加物

反応条件

温度: 100 °C

実験手順

To a solution of 0.945 g (3.18 mmol) of 7-(6-phenylhexyl)-5,6,7,8-tetrahydro-4H-furo[2,3-c]azepine in 20 ml of acetic acid, 0.34 g (3.8 mmol) of 50% aqueous dimethylamine and 0.31 g (3.8 mmol) of 37% aqueous formaldehyde were added, followed by stirring at 100° C. for 30 minutes. After the solvent was distilled off under reduced pressure, the residual solution was alkalified with aqueous sodium hydroxide and extracted with dichloromethane 3 times. The combined organic layer was dried over anhydrous magnesium sulfate; the solvent was distilled off under reduced pressure. The resulting crude product was purified by silica gel column chromatography (ethyl acetate to ethyl acetate/methanol=4/1) to yield the desired product.