Formamide → HCID 3041177、化合物

反応式

[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH2:11][CH2:12][C:13](=O)[CH3:14])[CH:6]=[CH:7][C:8]=1[O:9][CH3:10].C([NH2:18])=O.[OH-].[Na+]>O>[NH2:18][CH:13]([CH2:12][CH2:11][C:5]1[CH:6]=[CH:7][C:8]([O:9][CH3:10])=[C:3]([O:2][CH3:1])[CH:4]=1)[CH3:14]

参加物

反応条件

温度: 210 °C

実験手順

A mixture of 41.4 g of 4-(3,4-dimethoxy-phenyl)-2-butanone and 41.9 ml of formamide is heated at 210° C. for 20 hours, cooled to ambient, 104 ml of 10N sodium hydroxide is added and the reaction mixture heated at reflux temperature for 24 hours. The reaction is cooled, added to 200 ml of water and extracted with diethyl ether. The diethyl ether solution is washed with 10% hydrochloric acid. The aqueous layer is made basic and extracted with diethyl ether. The organic layer is dried, filtered and evaporated in vacuo. The residue is purified by chromatography (silica gel: chloroform/hexane/ethyl acetate to 5% methyl alcohol/chrloroform) to give 5.72 g of racemic 2 -amino-4 -(3,4-dimethoxyphenyl)butane.