Hydrochloric Acid → 2-[5-(5-Chloro-thiophen-2-yl)-isoxazol-3-ylmethyl]-5-thiophen-2-yl-2H-pyrazole-3-carboxylic acid

HRID 33234Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 33234
C([O:3][C:4]([C:6]1[N:7]([CH2:16][C:17]2[CH:21]=[C:20]([C:22]3[S:23][C:24]([Cl:27])=[CH:25][CH:26]=3)[O:19][N:18]=2)[N:8]=[C:9]([C:11]2[S:12][CH:13]=[CH:14][CH:15]=2)[CH:10]=1)=[O:5])C.O.[OH-].[Li+].Cl>C1COCC1.O>[Cl:27][C:24]1[S:23][C:22]([C:20]2[O:19][N:18]=[C:17]([CH2:16][N:7]3[C:6]([C:4]([OH:5])=[O:3])=[CH:10][C:9]([C:11]4[S:12][CH:13]=[CH:14][CH:15]=4)=[N:8]3)[CH:21]=2)=[CH:26][CH:25]=1

Komponenten

6

Edukt 3

HCID 313Hydrochloric AcidHCID 168937Lithium hydroxide, monohydrateHCID 121509052-[5-(5-Chloro-thiophen-2-yl)-isoxazol-3-ylmethyl]-5-thiophen-2-yl-2H-pyrazole-3-carboxylic acid ethyl ester

Produkt 1

HCID 121509062-[5-(5-Chloro-thiophen-2-yl)-isoxazol-3-ylmethyl]-5-thiophen-2-yl-2H-pyrazole-3-carboxylic acid

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 8028TetrahydrofuranLösungsmittel

Reaktionsbedingungen

Temperatur
60 °C

Versuchsvorschrift

To a solution of 4 g 2-[5-(5-Chloro-thiophen-2-yl)-isoxazol-3-ylmethyl]-5-thiophen-2-yl-2H-pyrazole-3-carboxylic acid ethyl ester in 20 ml THF, 10 ml water and 500 mg lithium hydroxide monohydrate were added. After stirring for 2 h at 60° C. the reaction was cooled to RT. The mixture was acidified with half concentrated hydrochloric acid to pH 3 and the precipitate collected by filtration and washed with 10 ml water The product was obtained as a white solid which was dried under reduced pressure.

Aufarbeitung

  1. temperaturewas cooled to RT
  2. filtrationthe precipitate collected by filtration
  3. washwashed with 10 ml water The product
  4. customwas obtained as a white solid which
  5. customwas dried under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-47f867ce9a484fc8a696a6c7980a2e20
Quelldatensatz
uspto-grants-2008_09
Patentnummer
US07429581B2

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