Lithium hydroxide, monohydrate → HCID 178524946, Verbindung

HRID 659797Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 659797
C([O:3][C:4]([C:6]1[C:10]([C:11]2[CH:16]=[CH:15][C:14]([Cl:17])=[CH:13][C:12]=2[Cl:18])=[CH:9][NH:8][N:7]=1)=[O:5])C.O.[OH-].[Li+]>C1COCC1.O>[Cl:18][C:12]1[CH:13]=[C:14]([Cl:17])[CH:15]=[CH:16][C:11]=1[C:10]1[C:6]([C:4]([OH:5])=[O:3])=[N:7][NH:8][CH:9]=1

Komponenten

4

Edukt 2

HCID 168937Lithium hydroxide, monohydrateHCID 178470487HCID 178470487, Verbindung

Produkt 1

HCID 178524946HCID 178524946, VerbindungAusbeute 108,1 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 21881883Oxolane--water (1/1)Lösungsmittel

Versuchsvorschrift

A solution of 4-(2,4-dichloro-phenyl)-1H-pyrazole-3-carboxylic acid ethyl ester (205 mg; 0.72 mmol) and lithium hydroxide monohydrate (125 mg; 2.9 mmol) in 1:1 THF/water (10 ml) was heated at 60° C. overnight. The THF was removed by evaporation, the aqueous phase acidified with 1M hydrochloric acid then extracted with ethyl acetate (20 ml). The ethyl acetate layer was dried (MgSO4), filtered and evaporated to give 200 mg of 4-(2,4-dichloro-phenyl)-1H-pyrazole-3-carboxylic acid. (LC/MS: [M+H]+ 256.85).

Aufarbeitung

  1. customThe THF was removed by evaporation
  2. extractionthen extracted with ethyl acetate (20 ml)
  3. dry with materialThe ethyl acetate layer was dried (MgSO4)
  4. filtrationfiltered
  5. customevaporated

Quellen und Nachweise

ORD-Eintrag
ord-81eaf89f066640fe9a3186a1daef1578
Quelldatensatz
uspto-grants-2011_12
Patentnummer
US08080666B2

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