Potassium Carbonate → HCID 21288084, Verbindung

HRID 868212Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 868212
[OH:1][C:2]1[CH:3]=[C:4]([C:7]([O:9][CH3:10])=[O:8])[S:5][CH:6]=1.Cl.Cl[CH2:13][C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][N:15]=1.C(=O)([O-])[O-].[K+].[K+]>CC(=O)CC>[N:15]1[CH:16]=[CH:17][CH:18]=[CH:19][C:14]=1[CH2:13][O:1][C:2]1[CH:3]=[C:4]([C:7]([O:9][CH3:10])=[O:8])[S:5][CH:6]=1

Komponenten

5

Edukt 3

HCID 11430Potassium CarbonateHCID 23392Picolyl chloride hydrochlorideHCID 13277908Methyl 4-hydroxythiophene-2-carboxylate

Produkt 1

HCID 21288084HCID 21288084, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6569Methyl Ethyl KetoneLösungsmittel

Versuchsvorschrift

3.00 g (19.0 mmol) of methyl 4-hydroxy-2-thiophenecarboxylate, 3.11 g (19.0 mmol) of 2-chloromethylpyridine hydrochloride and 5.24 g (37.9 mmol) of potassium carbonate are heated under reflux in 60 ml of absolute 2-butanone for 10 hours under nitrogen. The mixture is then evaporated in vacuo and the residue is partitioned between methylene chloride and saturated sodium bicarbonate solution. The aqueous phase is extracted twice more with 100 ml of methylene chloride each time and the combined organic phases are dried over sodium sulfate/active charcoal, filtered and evaporated. The residue is digested with diisopropyl ether.

Aufarbeitung

  1. customThe mixture is then evaporated in vacuo
  2. customthe residue is partitioned between methylene chloride and saturated sodium bicarbonate solution
  3. extractionThe aqueous phase is extracted twice more with 100 ml of methylene chloride each time
  4. dry with materialthe combined organic phases are dried over sodium sulfate/active charcoal
  5. filtrationfiltered
  6. customevaporated

Quellen und Nachweise

ORD-Eintrag
ord-173754239b17438095e56780c90626e7
Quelldatensatz
uspto-grants-1988_10
Patentnummer
US04778803

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