Isoquinoline → 2-Aminoisoquinolinium Iodide

HRID 1036640

Reaktionsgleichung

Reaktionsgleichung von HRID 1036640
[NH2:1]OS(O)(=O)=O.[CH:7]1[C:16]2[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=2)[CH:10]=[CH:9][N:8]=1.C(=O)([O-])[O-].[K+].[K+].[IH:23]>O>[I-:23].[NH2:1][N+:8]1[CH:9]=[CH:10][C:11]2[C:16](=[CH:15][CH:14]=[CH:13][CH:12]=2)[CH:7]=1

Komponenten

6

Edukt 4

HCID 8405IsoquinolineHCID 11430Potassium CarbonateHCID 24841Hydrogen iodideHCID 76284hydroxylamine-O-sulfonic acid

Produkt 1

HCID 108586012-Aminoisoquinolinium Iodide

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

A solution of hydroxylamine-O-sulfonic acid (2) (2 g, 1 equiv), water (10 mL) and isoquinoline (1) (6.3 mL, 3 equiv) was heated at 90° C. for 2-3 h. Potassium carbonate (2.44 g, 1 equiv) was added, and the water was evaporated. Ethanol (20-30 mL) was added to the solid residue, and insoluble potassium sulfate was filtered out. Hydroiodic acid (57%-67%, 1.34 mL, 1 equiv) was added to the filtrate, and the resulting solution was placed in a freezer. The precipitate was filtered out, washed with ethanol, and dried in vacuo. Isolated products were used as such in further reactions. Yield of the product was 1.78 g.

Aufarbeitung

  1. customthe water was evaporated
  2. additionEthanol (20-30 mL) was added to the solid residue, and insoluble potassium sulfate
  3. filtrationwas filtered out
  4. filtrationThe precipitate was filtered out
  5. washwashed with ethanol
  6. customdried in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-f8ce45c2a6ab4a57bf8d7f94db905dd5
Quelldatensatz
uspto-grants-2013_10
Patentnummer
US08546426B2

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