Acetonitrile → 1-Propanone, 3-(dimethylamino)-2-[(dimethylamino)methyl]-1-phenyl-

HRID 414158

반응식

HRID 414158 반응식
[Cl-].C[CH:3]=[N+:4]=[CH:5]C.[CH3:7][N:8]([CH3:19])[CH2:9][CH2:10][C:11]([C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1)=[O:12].[C:20](#N)C>>[CH3:19][N:8]([CH3:7])[CH2:9][CH:10]([C:11](=[O:12])[C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1)[CH2:3][N:4]([CH3:5])[CH3:20]

참가 물질

4

반응물 3

HCID 6342AcetonitrileHCID 770423-(Dimethylamino)-1-phenyl-1-propanoneHCID 21873455N,N-dimethylmethylene ammonium chloride

생성물 1

HCID 4329041-Propanone, 3-(dimethylamino)-2-[(dimethylamino)methyl]-1-phenyl-

실험 절차

The compound N,N,N',N'-tetramethyl-2-benzoyl-1,3-propanediamine (VIII) was synthesized by the method of Kinast and Tietze, Angew. Chemie. Int. Ed. 15 239-240 (1976). A mixture of 500 parts of N,N-dimethylmethylene ammonium chloride, 2600 parts of dry acetonitrile and 1035 parts of compound VII, described above, was heated to reflux under nitrogen for 15 minutes. The mixture was allowe to cool to room temperature andd then placed in the refrigerator overnight. A total of 800 parts of the hydrochloride salt of VI was isolated by filtration. The mother liquor was made basic with 10% NaOH solution and extracted with ether, the ether solution dried with anhydrous potassium carbonate and the ether evaporated under reduced pressure to yield 479 parts of a light yellow, low melting solid identified as VIII by NMR spectroscopy. The total yield of VIII was thus 93%.

후처리

  1. temperaturewas heated
  2. temperatureto reflux under nitrogen for 15 minutes
  3. customplaced in the refrigerator overnight

출처 및 근거

ORD 기록
ord-b17ba8dc4b7044289d4c9e07c09834b9
출처 데이터셋
uspto-grants-1988_12
특허 번호
US04791045

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