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HCID 14722309, Verbindung → HCID 10620577, Verbindung

HRID 1031680
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1031680
C([O:8][C:9]1[CH:22]=[C:21]([NH:23][S:24]([CH3:27])(=[O:26])=[O:25])[C:20]([O:28][C:29]2[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=2)=[CH:19][C:10]=1[C:11]([CH2:13][C:14]([O:16][CH2:17][CH3:18])=[O:15])=[O:12])C1C=CC=CC=1>C(O)C.[C].[Pd]>[OH:8][C:9]1[CH:22]=[C:21]([NH:23][S:24]([CH3:27])(=[O:26])=[O:25])[C:20]([O:28][C:29]2[CH:30]=[CH:31][CH:32]=[CH:33][CH:34]=2)=[CH:19][C:10]=1[C:11]([CH2:13][C:14]([O:16][CH2:17][CH3:18])=[O:15])=[O:12]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 1

HCID 14722309HCID 14722309, Verbindung

Produkt 1

HCID 10620577HCID 10620577, VerbindungAusbeute 88 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 178418390HCID 178418390, VerbindungKatalysatorHCID 702EthanolLösungsmittel

Versuchsvorschrift

In 50 ml of ethanol was dissolved 4.83 g of ethyl 2-(2-benzyloxy-4-methylsulfonylamino-5-phenoxybenzoyl)acetate. Thereto was added 200 mg of 5% palladium-carbon. The mixture was subjected to hydrogenation for 1 hour at 40° C. at atmospheric pressure. After the completion of the reaction, the catalyst was removed by filtration. The filtrate was subjected to distillation under reduced pressure to remove the solvent. The residue was mixed with diisopropyl ether. The resulting crystal was collected by filtration and recrystallized from a mixed solvent of ethyl acetate and diisopropyl ether to obtain 3.46 g (yield: 88%) of ethyl 2-(2-hydroxy-4-methylsulfonylamino-5-phenoxybenzoyl)acetate having a melting point of 111.5°-112.5° C.

Aufarbeitung

  1. customAfter the completion of the reaction
  2. customthe catalyst was removed by filtration
  3. distillationThe filtrate was subjected to distillation under reduced pressure
  4. customto remove the solvent
  5. additionThe residue was mixed with diisopropyl ether
  6. filtrationThe resulting crystal was collected by filtration
  7. customrecrystallized from a mixed solvent of ethyl acetate and diisopropyl ether

Quellen und Nachweise

ORD-Eintrag
ord-1eed135637b34bfcba7753e0594d2d0b
Quelldatensatz
uspto-grants-1990_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04954518

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