Acetic Acid → HCID 14622774, Verbindung

HRID 1721937Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1721937
S1C=CC=C1CC([O-])=O.[K+].[Cl:11][C:12]1[C:17]([Cl:18])=[C:16]([O:19]C)[CH:15]=[CH:14][C:13]=1[C:21]([C:23]1[N:27]([CH2:28][O:29][CH2:30][CH3:31])[N:26]=[CH:25][CH:24]=1)=[O:22].O.C(O)(=O)C>CS(C)=O>[Cl:18][C:17]1[C:12]([Cl:11])=[C:13]([C:21]([C:23]2[N:27]([CH2:28][O:29][CH2:30][CH3:31])[N:26]=[CH:25][CH:24]=2)=[O:22])[CH:14]=[CH:15][C:16]=1[OH:19]

Komponenten

6

Edukt 4

HCID 176Acetic AcidHCID 962WaterHCID 14622785HCID 14622785, VerbindungHCID 23696799Potassium 2-thienylacetate

Produkt 1

HCID 14622774HCID 14622774, VerbindungAusbeute 71,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 679Dimethyl SulfoxideLösungsmittel

Versuchsvorschrift

9.45 g of potassium thiolacetate are added to a solution of 5.45 g of (2,3-dichloro-4-methoxyphenyl)(1-ethoxymethyl-5-pyrazolyl)methanone in dimethylsulfoxide and the mixture is stirred at 90°-100° C. under argon gas atmosphere for 4 hours. After cooling the solution, cold water is added thereto, and the mixture is adjusted to pH 5-6 with acetic acid and then extracted with ethyl acetate. The extract is washed with water, dried and evaporated to remove solvent. The residue is purified by silica gel column chromatography to give 3.72 g of 2,3-dichloro-4-(1-ethoxymethyl-5-pyrazolylcarbonyl)phenol.

Aufarbeitung

  1. additionis added
  2. extractionextracted with ethyl acetate
  3. washThe extract is washed with water
  4. customdried
  5. customevaporated
  6. customto remove solvent
  7. customThe residue is purified by silica gel column chromatography

Quellen und Nachweise

ORD-Eintrag
ord-aa4f7bde85d64daa844eb84d52806c60
Quelldatensatz
uspto-grants-1989_08
Patentnummer
US04853404

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