Potassium Carbonate → HCID 14695585, Verbindung

HRID 619893Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 619893
[F:1][C:2]1[CH:7]=[C:6]([Cl:8])[C:5]([O:9]C(OC)=O)=[CH:4][C:3]=1[N:14]1[C:18](=[O:19])[C:17](=[C:20]([CH3:22])[CH3:21])[O:16][C:15]1=[O:23].C(=O)([O-])[O-].[K+].[K+]>CO>[F:1][C:2]1[CH:7]=[C:6]([Cl:8])[C:5]([OH:9])=[CH:4][C:3]=1[N:14]1[C:18](=[O:19])[C:17](=[C:20]([CH3:21])[CH3:22])[O:16][C:15]1=[O:23]

Komponenten

4

Edukt 2

HCID 11430Potassium CarbonateHCID 14695618HCID 14695618, Verbindung

Produkt 1

HCID 14695585HCID 14695585, VerbindungAusbeute 56 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

To a dried methanol solution (100 ml) of 3-(2'-fluoro-4'-chloro-5'-methoxycarbonyloxyphenyl)-5-isopropylidene-1,3-oxazolidine-2,4-dione (3.44 g, 10 mmol), which was synthesized by a method shown in Reference Example 12 described below, was added potassium carbonate (1.38 g, 10 mmol) and the mixture was heated at reflux for 2 hours. After the reaction was completed, the resulting mixture was quenched with an aqueous solution of ammonium chloride and extracted with ether. The ethereal extracts were dried and evaporated as small a volume as possible. The resulting residue was purified by silica gel column chromatography to give pure 3-(2'-fluoro-4'-chloro-5'-hydroxyphenyl)-5-isopropylidene-1,3-oxazolidine-2,4-dione (1.60 g).

Aufarbeitung

  1. temperaturethe mixture was heated
  2. temperatureat reflux for 2 hours
  3. customthe resulting mixture was quenched with an aqueous solution of ammonium chloride
  4. extractionextracted with ether
  5. customThe ethereal extracts were dried
  6. customevaporated as small a volume as possible
  7. customThe resulting residue was purified by silica gel column chromatography

Quellen und Nachweise

ORD-Eintrag
ord-60e8a624e39c4e308aea2683648e23c4
Quelldatensatz
uspto-grants-1989_04
Patentnummer
US04818272

Notizen zur Reaktion

Wird geladen…