反応式
[C:1]([C:4]1[S:5][CH:6]=[CH:7][CH:8]=1)(=[O:3])[CH3:2].[ClH:9].[CH3:10][NH:11][CH3:12].[CH2:13]=O.Cl>C(O)C.CC(C)=O>[ClH:9].[CH3:10][N:11]([CH3:13])[CH2:12][CH2:2][C:1]([C:4]1[S:5][CH:6]=[CH:7][CH:8]=1)=[O:3]参加物
7
実験手順
A mixture of 2-acetylthiophene (63.1 g, 0.5 mol), dimethylamine hydrochloride (53.0 g, 0.65 mol), paraformaldehyde (19.8 g, 0.22 mol), and 12N hydrochloric acid (1 ml) in ethanol (80 ml) was refluxed for one and one-half hours. The solution was diluted with ethanol (100 ml) and acetone (500 ml). The solution was chilled overnight and the resulting solid was collected by filtration to yield 75.0 g (73%) of 3-dimethylamino-1-(2-thienyl)-1-propanone hydrochloride as a colorless crystalline solid. mp =182° C.-184° C.
後処理
- temperaturewas refluxed for one and one-half hours
- temperatureThe solution was chilled overnight
- filtrationthe resulting solid was collected by filtration
出典と根拠
- ORDレコード
- ord-84ab1556f112429aa3c3af0c90e4d4a4
- 出典データセット
- uspto-grants-1991_06
- 特許番号
- US05023269
関連ノート
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