Hydrochloric Acid → 1-Propanone, 3-(dimethylamino)-1-phenyl-, hydrochloride (1:1)
反応式
[C:1]([C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1)(=[O:3])[CH3:2].[CH2:10]=O.[ClH:12].[CH3:13][NH:14][CH3:15].Cl>C(O)C.CC(C)=O>[ClH:12].[CH3:13][N:14]([CH3:10])[CH2:15][CH2:2][C:1]([C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1)=[O:3]参加物
7
実験手順
Acetophenone (29.1 ml, 0.25 mol), para-formaldehyde (12.0 g, 0.40 mol) and dimethyl amine hydrochloride (28.5 g, 0.35 mol) are suspended in ethanol (50 ml). Concentrated hydrochloric acid (0.5 ml) is added and the mixture is heated to reflux for 4 h. Then acetone (200 ml) is added and the resulting clear solution is allowed to cool to ambient temperature. The precipitate is collected by filtration and crystallized from ethanol yielding the title compound (40.7 g, 76.0% of theoretical yield) as colorless crystals with mp. 158° C.
後処理
- temperaturethe mixture is heated
- temperatureto reflux for 4 h
- filtrationThe precipitate is collected by filtration
- customcrystallized from ethanol yielding the title compound (40.7 g, 76.0% of theoretical yield) as colorless crystals with mp. 158° C.
出典と根拠
- ORDレコード
- ord-ab050129ebc54d3b8ce218ab6033913d
- 出典データセット
- uspto-grants-1998_10
- 特許番号
- US05824624
反応ノート
読み込み中…