Potassium Carbonate → HCID 13386244, Verbindung

HRID 647445

Reaktionsgleichung

Reaktionsgleichung von HRID 647445
Cl[C:2]1[N:3]=[CH:4][C:5]2[C:10]([CH:11]=1)=[CH:9][CH:8]=[C:7]([Cl:12])[CH:6]=2.[CH3:13][O:14][C:15]1[CH:21]=[CH:20][C:18]([O-:19])=[CH:17][CH:16]=1.[Na+].C(=O)([O-])[O-].[K+].[K+]>[Cu]=O>[Cl:12][C:7]1[CH:6]=[C:5]2[C:10]([CH:11]=[C:2]([O:19][C:18]3[CH:20]=[CH:21][C:15]([O:14][CH3:13])=[CH:16][CH:17]=3)[N:3]=[CH:4]2)=[CH:9][CH:8]=1

Komponenten

5

Edukt 3

HCID 11430Potassium CarbonateHCID 204849213,7-DichloroisoquinolineHCID 23679016Sodium 4-methoxyphenolate

Produkt 1

HCID 13386244HCID 13386244, VerbindungAusbeute 45,9 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 14829Copper oxideKatalysator

Reaktionsbedingungen

Temperatur
180 °C

Versuchsvorschrift

A mixture of 3,7-dichloroisoquinoline (5.59 g), sodium 4-methoxyphenoxide (4.55 g), potassium carbonate (3.86 g) copper powder (50 mg) and trace of copper oxide were heated at 180° C. for 14 hrs. the mixture was then cooled and extracted with ethyl acetate, which in turn was washed with water, dried (MgSO4) and evaporated to give a crude brown solid. Purification by column chromatography over silica gel gave 7-chloro-3-(4-methoxyphenoxy)isoquinoline (3.70 g) as a tan solid, mp 77° C.

Aufarbeitung

  1. temperaturethe mixture was then cooled
  2. extractionextracted with ethyl acetate, which in turn
  3. washwas washed with water
  4. dry with materialdried (MgSO4)
  5. customevaporated
  6. customto give a crude brown solid
  7. customPurification by column chromatography over silica gel

Quellen und Nachweise

ORD-Eintrag
ord-8d2791673b6a49dca3f82dd22017e54f
Quelldatensatz
uspto-grants-1983_10
Patentnummer
US04409017

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