N,N-Diethylethylenediamine → HCID 21486957, Verbindung

HRID 1414278Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1414278
[CH2:1]([N:3]([CH2:7][CH3:8])[CH2:4][CH2:5][NH2:6])[CH3:2].[CH3:9][O:10][C:11]1[CH:12]=[C:13]2[C:18](=[CH:19][C:20]=1[O:21][CH3:22])[CH:17]([C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1)[N:16]([C:29](Cl)=[O:30])[CH2:15][CH2:14]2>O>[CH2:1]([N:3]([CH2:7][CH3:8])[CH2:4][CH2:5][NH:6][C:29]([N:16]1[CH2:15][CH2:14][C:13]2[C:18](=[CH:19][C:20]([O:21][CH3:22])=[C:11]([O:10][CH3:9])[CH:12]=2)[CH:17]1[C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1)=[O:30])[CH3:2]

Komponenten

4

Edukt 2

HCID 60993N,N-DiethylethylenediamineHCID 214870076,7-dimethoxy-1-phenyl-3,4-dihydro-2(1H)-isoquinolinecarbonyl chloride

Produkt 1

HCID 21486957HCID 21486957, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

To 10 parts by volume of 2-diethylaminoethylamine is added 3.0 parts of 6,7-dimethoxy-1-phenyl-3,4-dihydro-2(1H)-isoquinolinecarbonyl chloride. An exothermic reaction ensues. The mixture is heated over a steam bath for approximately 30 minutes. (Alternatively, the mixture is maintained at room temperature overnight.) The reaction mixture is then poured into water and extracted with ethyl ether. The ether layer is dried over anhydrous calcium sulfate and evaporated to dryness. The solid thus obtained is crystallized from a mixture of ethyl ether and n-hexane to afford N-(2-diethylaminoethyl)-6,7-dimethoxy-1-phenyl-3,4-dihydro-2(1H)-isoquinolinecarboxamide, melting at about 97°-98°C.

Aufarbeitung

  1. customAn exothermic reaction
  2. temperatureThe mixture is heated over a steam bath for approximately 30 minutes
  3. extractionextracted with ethyl ether
  4. dry with materialThe ether layer is dried over anhydrous calcium sulfate
  5. customevaporated to dryness
  6. customThe solid thus obtained
  7. customis crystallized from a mixture of ethyl ether and n-hexane

Quellen und Nachweise

ORD-Eintrag
ord-78f928b92249456fb86c9502fac5b461
Quelldatensatz
uspto-grants-1977_01
Patentnummer
US04001244

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