Dimethylamine → HCID 23467112, Verbindung

HRID 443385Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 443385
[Cl:1][C:2]1[N:3]=[C:4]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[C:5]2[C:10]([C:11]=1[CH2:12]O)=[CH:9][CH:8]=[CH:7][CH:6]=2.P(Br)(Br)Br.[CH3:24][NH:25][CH3:26]>C1(C)C=CC=CC=1>[Cl:1][C:2]1[N:3]=[C:4]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[C:5]2[C:10]([C:11]=1[CH2:12][N:25]([CH3:26])[CH3:24])=[CH:9][CH:8]=[CH:7][CH:6]=2

Komponenten

5

Edukt 3

HCID 674DimethylamineHCID 24614Phosphorus tribromideHCID 14567249HCID 14567249, Verbindung

Produkt 1

HCID 23467112HCID 23467112, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel

Versuchsvorschrift

8.2 g 3-Chloro-4-hydroxymethyl-1-phenyl-isoquinoline are suspended in 300 ml toluene and 16.2 g phosphorus tribromide are added thereto while cooling with ice. After a 10 hours' stirring at room temperature dimethylamine is introduced until an alcaline reaction occurs. The reaction mixture is concentrated and water is added to the residue. Extraction with acetic acid ester gives a yellow oil, that crystallizes slowly. Melting point 75° to 77° C. Hydrochloride: 244° to 246° C.

Aufarbeitung

  1. temperaturewhile cooling with ice
  2. additionis introduced until an alcaline reaction
  3. concentrationThe reaction mixture is concentrated
  4. additionwater is added to the residue
  5. extractionExtraction with acetic acid ester
  6. customgives a yellow oil
  7. customthat crystallizes slowly
  8. custom244° to 246° C.

Quellen und Nachweise

ORD-Eintrag
ord-2ab48a7df67248e08a4c8f832868e09a
Quelldatensatz
uspto-grants-1981_04
Patentnummer
US04260611

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