1,2-Ethanediamine, N1,N1-bis(1-methylethyl)- → N-(2-diisopropylaminoethyl)-6,7-dimethoxy-1-(3,4-dimethoxyphenyl)-3,4-dihydro-2(1H)-isoquinolinecarboxamide

HRID 1414283

Reaktionsgleichung

Reaktionsgleichung von HRID 1414283
[CH:1]([N:4]([CH:8]([CH3:10])[CH3:9])[CH2:5][CH2:6][NH2:7])([CH3:3])[CH3:2].[CH3:11][O:12][C:13]1[CH:14]=[C:15]2[C:20](=[CH:21][C:22]=1[O:23][CH3:24])[CH:19]([C:25]1[CH:30]=[CH:29][C:28]([O:31][CH3:32])=[C:27]([O:33][CH3:34])[CH:26]=1)[N:18]([C:35](Cl)=[O:36])[CH2:17][CH2:16]2.C(N(CC)CC)C>C(Cl)(Cl)Cl>[CH:1]([N:4]([CH:8]([CH3:10])[CH3:9])[CH2:5][CH2:6][NH:7][C:35]([N:18]1[CH2:17][CH2:16][C:15]2[C:20](=[CH:21][C:22]([O:23][CH3:24])=[C:13]([O:12][CH3:11])[CH:14]=2)[CH:19]1[C:25]1[CH:30]=[CH:29][C:28]([O:31][CH3:32])=[C:27]([O:33][CH3:34])[CH:26]=1)=[O:36])([CH3:3])[CH3:2]

Komponenten

5

Edukt 3

HCID 84591,2-Ethanediamine, N1,N1-bis(1-methylethyl)-HCID 8471TriethylamineHCID 214869646,7-dimethoxy-1-(3,4-dimethoxyphenyl)-3,4-dihydro-2(1H)-isoquinolinecarbonyl chloride

Produkt 1

HCID 21487010N-(2-diisopropylaminoethyl)-6,7-dimethoxy-1-(3,4-dimethoxyphenyl)-3,4-dihydro-2(1H)-isoquinolinecarboxamide

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6212ChloroformLösungsmittel2×

Versuchsvorschrift

4.0 Parts of 2-diisopropylaminoethylamine in 75 parts of chloroform is added portionwise, at room temperature, to a mixture of 8.0 parts of 6,7-dimethoxy-1-(3,4-dimethoxyphenyl)-3,4-dihydro-2(1H)-isoquinolinecarbonyl chloride and 15 parts of triethylamine in 225 parts of chloroform. After the addition is complete, the mixture is stirred for 3 to 4 hours, allowed to stand overnight, and then washed with water. The chloroform layer is separated, dried over anhydrous calcium sulfate and concentrated under reduced pressure. The solid material obtained in this manner is crystallized from ether to give N-(2-diisopropylaminoethyl)-6,7-dimethoxy-1-(3,4-dimethoxyphenyl)-3,4-dihydro-2(1H)-isoquinolinecarboxamide, melting at about 114°-115°C.

Aufarbeitung

  1. additionAfter the addition
  2. waitto stand overnight
  3. washwashed with water
  4. customThe chloroform layer is separated
  5. dry with materialdried over anhydrous calcium sulfate
  6. concentrationconcentrated under reduced pressure
  7. customThe solid material obtained in this manner
  8. customis crystallized from ether

Quellen und Nachweise

ORD-Eintrag
ord-3668809edd3f4ec5a21be884fe9ad38e
Quelldatensatz
uspto-grants-1977_01
Patentnummer
US04001244

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