Potassium Carbonate → HCID 21271267, Verbindung

HRID 1194008Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1194008
[OH:1][C:2]1[CH:3]=[C:4]([C:7]([O:9][CH3:10])=[O:8])[S:5][CH:6]=1.I[CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][C:19]1[O:23][N:22]=[C:21]([CH3:24])[CH:20]=1.C(=O)([O-])[O-].[K+].[K+]>CC(C)=O>[CH3:24][C:21]1[CH:20]=[C:19]([CH2:18][CH2:17][CH2:16][CH2:15][CH2:14][CH2:13][CH2:12][O:1][C:2]2[CH:3]=[C:4]([C:7]([O:9][CH3:10])=[O:8])[S:5][CH:6]=2)[O:23][N:22]=1

Komponenten

5

Edukt 3

HCID 11430Potassium CarbonateHCID 13277908Methyl 4-hydroxythiophene-2-carboxylateHCID 21271268HCID 21271268, Verbindung

Produkt 1

HCID 21271267HCID 21271267, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 180AcetoneLösungsmittel

Versuchsvorschrift

6.42 g (40.60 mmol) of methyl 4-hydroxy-2-thiophenecarboxylate (XIa) and 11.88 g (38.67 mmol) of 5-(7-iodoheptyl)-3-methyl-isoxazole (IX) are heated under reflux with 5.34 g (40.60 mmol) of potassium carbonate (K2CO3) in 130 ml of anhydrous acetone for 8 hours. After the mixture has been left to stand overnight, it is concentrated, the residue is partitioned between 2N NaOH and ether and the aqueous phase is extracted several times with a total of 150 ml of ether. The organic phase is dried over sodium sulfate/active charcoal and evaporated.

Aufarbeitung

  1. waitAfter the mixture has been left
  2. concentrationit is concentrated
  3. customthe residue is partitioned between 2N NaOH and ether
  4. extractionthe aqueous phase is extracted several times with a total of 150 ml of ether
  5. dry with materialThe organic phase is dried over sodium sulfate/active charcoal
  6. customevaporated

Quellen und Nachweise

ORD-Eintrag
ord-d1919189db3f431594790d2f33c6fc7a
Quelldatensatz
uspto-grants-1989_03
Patentnummer
US04812472

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