HCID 178470495, Verbindung → HCID 178524954, Verbindung

HRID 20310

Reaktionsgleichung

Reaktionsgleichung von HRID 20310
C([O:3][C:4]([C:6]1[C:10]([NH:11][C:12](=[O:21])[C:13]2[C:18]([F:19])=[CH:17][CH:16]=[CH:15][C:14]=2[F:20])=[CH:9][NH:8][N:7]=1)=[O:5])C>[OH-].[Na+].CO>[F:19][C:18]1[CH:17]=[CH:16][CH:15]=[C:14]([F:20])[C:13]=1[C:12]([NH:11][C:10]1[C:6]([C:4]([OH:5])=[O:3])=[N:7][NH:8][CH:9]=1)=[O:21]

Komponenten

3

Edukt 1

HCID 178470495HCID 178470495, Verbindung

Produkt 1

HCID 178524954HCID 178524954, VerbindungAusbeute 61,7 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 23721981Sodium hydroxide methanolLösungsmittel

Versuchsvorschrift

A mixture of 4-(2,6-difluoro-benzoylamino)-1H-pyrazole-3-carboxylic acid ethyl ester (10.2 g) in 2 M aqueous NaOH/MeOH (1:1, 250 ml) was stirred at ambient temperature for 14 h. Volatile materials were removed in vacuo, water (300 ml) added and the mixture taken to pH 5 using 1M aqueous HCl. The resultant precipitate was collected by filtration and dried through azeotrope with toluene to afford 4-(2,6-difluoro-benzoylamino)-1H-pyrazole-3-carboxylic acid as a pink solid (5.70 g). (LC/MS: Rt 2.33, [M+H]+ 267.96).

Aufarbeitung

  1. customVolatile materials were removed in vacuo, water (300 ml)
  2. additionadded
  3. filtrationThe resultant precipitate was collected by filtration
  4. dry with materialdried through azeotrope with toluene

Quellen und Nachweise

ORD-Eintrag
ord-585e59fc6d6949348d8df84c97e249de
Quelldatensatz
uspto-grants-2010_06
Patentnummer
US07745638B2

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