Methanol → HCID 68878024, Verbindung

HRID 1436011

Reaktionsgleichung

Reaktionsgleichung von HRID 1436011
[Cl:1]C1C=CC=C(C(OO)=[O:9])C=1.[Br:12][C:13]1[C:22]([O:23][CH3:24])=[CH:21][CH:20]=[C:19]2[C:14]=1[CH:15]=[CH:16][N:17]=[CH:18]2.CO>ClCCl>[ClH:1].[Br:12][C:13]1[C:22]([O:23][CH3:24])=[CH:21][CH:20]=[C:19]2[C:14]=1[CH:15]=[CH:16][N+:17]([O-:9])=[CH:18]2

Komponenten

5

Edukt 3

HCID 887MethanolHCID 70297m-Chloroperbenzoic acidHCID 222265455-Bromo-6-methoxy-isoquinoline

Produkt 1

HCID 68878024HCID 68878024, VerbindungAusbeute 83,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel2×

Versuchsvorschrift

m-Chloroperbenzoic acid (1.4 g, 75%) was added in portions to a stirred solution of 5-bromo-6-methoxyisoquinoline (12 g, 5.04 mmol) in dichloromethane (12 ml). The mixture was stirred for 1 h then further dichloromethane (10 ml) added and the mixture stirred for an additional 2 h. Methanol (12 ml) was added and the mixture concentrated in vacuo to ˜9 ml, then 1M hydrochloric acid in diethyl ether (10 ml) was added. The mixture was diluted with ether and filtered, the precipitated solid was washed with diethyl ether and dried in vacuo to give crude 5-bromo-6-methoxyisoquinoline-N-oxide hydrochloride (1.22 g).

Aufarbeitung

  1. stirringthe mixture stirred for an additional 2 h
  2. concentrationthe mixture concentrated in vacuo to ˜9 ml
  3. addition1M hydrochloric acid in diethyl ether (10 ml) was added
  4. additionThe mixture was diluted with ether
  5. filtrationfiltered
  6. washthe precipitated solid was washed with diethyl ether
  7. customdried in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-a3cddaab01a94e84accae8268c62de9f
Quelldatensatz
uspto-grants-2009_11
Patentnummer
US07618985B2

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