Water → HCID 178460720, Verbindung

HRID 498953

Reaktionsgleichung

Reaktionsgleichung von HRID 498953
Cl[C:2]1[CH:11]=[C:10]([C:12]2[C:13]([C:17]([F:20])([F:19])[F:18])=[N:14][NH:15][CH:16]=2)[CH:9]=[CH:8][C:3]=1[C:4]([O:6][CH3:7])=[O:5].[CH2:21]([SH:24])[CH2:22][CH3:23].C(=O)([O-])[O-].[K+].[K+].O>CN(C)C=O>[CH2:21]([S:24][C:2]1[CH:11]=[C:10]([C:12]2[C:13]([C:17]([F:20])([F:19])[F:18])=[N:14][NH:15][CH:16]=2)[CH:9]=[CH:8][C:3]=1[C:4]([O:6][CH3:7])=[O:5])[CH2:22][CH3:23]

Komponenten

6

Edukt 4

HCID 962WaterHCID 7848Propyl mercaptanHCID 11430Potassium CarbonateHCID 178497552HCID 178497552, Verbindung

Produkt 1

HCID 178460720HCID 178460720, VerbindungAusbeute 18 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

1.52 g (5.0 mmol) of methyl 2-chloro-4-(3-trifluoromethylpyrazolyl)benzoate, 0.66 g (8.6 mmol) of 1-propanethiol and 0.83 g (6.0 mmol) of potassium carbonate were stirred in 5 ml of N,N-dimethylformamide at 60° C. for 24 hours. The resulting reaction mixture was poured into 50 ml of water, and the organic matters were extracted with 20 ml of ethyl acetate twice. The ethyl acetate layers were combined, washed with 30 ml of water twice and dried over anhydrous magnesium sulfate, and the ethyl acetate was distilled off under reduced pressure. Purification of the residue by thin layer chromatography afforded 0.31 g of methyl 2-propylthio-4-(3-trifluoromethylpyrazolyl)benzoate as a white powder (m.p. 114-116° C.).

Aufarbeitung

  1. customThe resulting reaction mixture
  2. extractionthe organic matters were extracted with 20 ml of ethyl acetate twice
  3. washwashed with 30 ml of water twice
  4. dry with materialdried over anhydrous magnesium sulfate
  5. distillationthe ethyl acetate was distilled off under reduced pressure
  6. customPurification of the residue by thin layer chromatography

Quellen und Nachweise

ORD-Eintrag
ord-2c5671f66d5d46b186019dbd66010b51
Quelldatensatz
uspto-grants-2010_08
Patentnummer
US07767626B2

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