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Sodium Hydroxide → HCID 86692504, Verbindung

HRID 1748557
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1748557
C([O:3][C:4]([C:6]1[CH:7]=[N:8][N:9]([C:12]2[C:17]([F:18])=[CH:16][C:15]([C:19]([F:22])([F:21])[F:20])=[CH:14][N:13]=2)[C:10]=1[CH3:11])=[O:5])C.[OH-].[Na+]>O1CCCC1>[F:18][C:17]1[C:12]([N:9]2[C:10]([CH3:11])=[C:6]([C:4]([OH:5])=[O:3])[CH:7]=[N:8]2)=[N:13][CH:14]=[C:15]([C:19]([F:22])([F:20])[F:21])[CH:16]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 14798Sodium HydroxideHCID 86692473HCID 86692473, Verbindung

Produkt 1

HCID 86692504HCID 86692504, VerbindungAusbeute 85,9 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

To a solution of 1-[3-fluoro-5-(trifluoromethyl)pyridin-2-yl]-5-methyl-1H-pyrazole-4-carboxylic acid ethyl ester (2.17 g) in tetrahydrofuran (10 ml) was added 1 N aqueous solution of sodium hydroxide (10 ml), and stirred at room temperature overnight. After completion of the reaction, the organic solvent was evaporated in vacuo, then water and diethyl ether were added thereto, and the aqueous layer was separated. To the aqueous layer was added 1 N hydrochloric acid aqueous solution under ice-cooling to adjust the layer to pH 5, the precipitated solid was collected by filtration, and dried at 60° C. under air blow to give the titled compound (1.7 g) as a white solid. MS (ESI) m/z: 290 (M+H)+.

Aufarbeitung

  1. customAfter completion of the reaction
  2. customthe organic solvent was evaporated in vacuo
  3. additionwater and diethyl ether were added
  4. customthe aqueous layer was separated
  5. additionTo the aqueous layer was added 1 N hydrochloric acid aqueous solution under ice-
  6. temperaturecooling
  7. filtrationthe precipitated solid was collected by filtration
  8. customdried at 60° C. under air blow

Quellen und Nachweise

ORD-Eintrag
ord-70cdd2f853f5418180de7090c7877b95
Quelldatensatz
uspto-grants-2015_10
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US09150555B2

Notizen zur Reaktion

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