Water → HCID 20433685, Verbindung

HRID 1154676

Reaktionsgleichung

Reaktionsgleichung von HRID 1154676
[CH3:1][O:2][C:3]1[C:14]([O:15][CH3:16])=[CH:13][C:6]2[CH2:7][C:8](=[O:12])[NH:9][CH2:10][CH2:11][C:5]=2[CH:4]=1.[Cl:17][CH2:18][CH2:19][CH2:20][N:21]([CH3:34])[CH2:22][CH2:23][C:24]1[CH:29]=[CH:28][C:27]([O:30][CH3:31])=[C:26]([O:32][CH3:33])[CH:25]=1.O>CS(C)=O>[ClH:17].[ClH:17].[CH3:1][O:2][C:3]1[C:14]([O:15][CH3:16])=[CH:13][C:6]2[CH2:7][C:8](=[O:12])[N:9]([CH2:18][CH2:19][CH2:20][N:21]([CH3:34])[CH2:22][CH2:23][C:24]3[CH:29]=[CH:28][C:27]([O:30][CH3:31])=[C:26]([O:32][CH3:33])[CH:25]=3)[CH2:10][CH2:11][C:5]=2[CH:4]=1

Komponenten

5

Edukt 3

HCID 962WaterHCID 577693N-(3-Chloropropyl)-3,4-dimethoxy-N-methylphenethylamineHCID 114017697,8-dimethoxy-2,3,4,5-tetrahydro-1H-3-benzazepin-2-one

Produkt 1

HCID 20433685HCID 20433685, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 679Dimethyl SulfoxideLösungsmittel

Versuchsvorschrift

1.1 gm (5.0 mmols) of 7,8-dimethoxy-1,3,4,5-tetrahydro-2H-3-benzazepin-2-one were suspended in 20 ml of dimethyl sulfoxide, and the suspension was mixed with 0.6 gm (5.3 mmols) of potassium tert. butylate while stirring. After 10 minutes, the solution was mixed with 2.0 gm (7.4 mmols) of 1-chloro-3-[N-methyl-N-(2-{3,4-dimethoxy-phenyl}-ethyl)-amino]-propane; the mixture was stirred for one hour at 50° C. and then poured into water; the aqueous mixture was extracted with ethyl acetate, and the organic phase was evaporated in vacuo. The residue was purified on silica gel with methylene chloride +10% of methanol as the eluant, and the dihydrochloride was precipitated from acetone with ethereal hydrochloric acid.

Aufarbeitung

  1. stirringthe mixture was stirred for one hour at 50° C.
  2. extractionthe aqueous mixture was extracted with ethyl acetate
  3. customthe organic phase was evaporated in vacuo
  4. customThe residue was purified on silica gel with methylene chloride +10% of methanol as the eluant
  5. customthe dihydrochloride was precipitated from acetone with ethereal hydrochloric acid

Quellen und Nachweise

ORD-Eintrag
ord-ad6624aec3ba45f5bf0598f0c6d817dc
Quelldatensatz
uspto-grants-1984_12
Patentnummer
US04490369

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