Hydrochloric Acid → 1-Propanone, 3-(dimethylamino)-1-phenyl-, hydrochloride (1:1)

HRID 399702

反応式

HRID 399702 の反応式
[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

反応物 4

HCID 313Hydrochloric AcidHCID 712FormaldehydeHCID 7410AcetophenoneHCID 10473Dimethylamine, hydrochloride

生成物 1

HCID 928441-Propanone, 3-(dimethylamino)-1-phenyl-, hydrochloride (1:1)

試薬・触媒・溶媒 2

HCID 180Acetone溶媒HCID 702Ethanol溶媒

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

  1. temperaturethe mixture is heated
  2. temperatureto reflux for 4 h
  3. filtrationThe precipitate is collected by filtration
  4. 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

関連ノート

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