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

HRID 399702

반응식

HRID 399702 반응식
[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]

참가 물질

7

반응물 4

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

생성물 1

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

시약·촉매·용매 2

HCID 180Acetone용매HCID 702Ethanol용매

실험 절차

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.

후처리

  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.

출처 및 근거

ORD 기록
ord-ab050129ebc54d3b8ce218ab6033913d
출처 데이터셋
uspto-grants-1998_10
특허 번호
US05824624

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