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1,4-Dioxane → HCID 15766694, Verbindung

HRID 1707583
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1707583
O1CCOCC1.[F:7][C:8]([F:24])([F:23])[C:9]1[C:10]([S:15]([NH:18][C:19](=[O:22])OC)(=[O:17])=[O:16])=[N:11][CH:12]=[CH:13][CH:14]=1.[CH3:25][C:26]1[CH2:30][CH:29]([C:31]2[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=2)[NH:28][N:27]=1>N1C=CC=CC=1>[F:23][C:8]([F:7])([F:24])[C:9]1[C:10]([S:15]([NH:18][C:19]([N:28]2[CH:29]([C:31]3[CH:32]=[CH:33][CH:34]=[CH:35][CH:36]=3)[CH2:30][C:26]([CH3:25])=[N:27]2)=[O:22])(=[O:16])=[O:17])=[N:11][CH:12]=[CH:13][CH:14]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 312751,4-DioxaneHCID 101301011H-Pyrazole, 4,5-dihydro-3-methyl-5-phenyl-HCID 15766693HCID 15766693, Verbindung

Produkt 1

HCID 15766694HCID 15766694, VerbindungAusbeute 82,4 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1049PyridineLösungsmittel

Versuchsvorschrift

A dry dioxane (10 ml) solution containing methyl N-(3-trifluoromethylpyridine-2-sulfonyl)carbamate (0.43 g, 1.5 mmol), 3-methyl-5-phenyl-2-pyrazoline (0.48 g, 3.0 mmol) and pyridine (0.45 g) was refluxed under heating and stirring for one hour. After cooling the mixture, the solvent was distilled off under reduced pressure, and the residue was stirred together with ethyl ether. Precipitated crystals were collected by filtration and then thoroughly washed with ethyl ether, and the crystals were suspended in 20 ml of water. Then, the pH was adjusted to a level of from 1 to 2 with concentrated hydrochloric acid, and the suspension was stirred at room temperature for 5 minutes. Crystals were collected by filtration, thoroughly washed with water and then with ethyl ether and dried to obtain 0.51 g of desired 1-(3-trifluoromethylpyridine-2-sulfonylcarbamoyl)-3-methyl-5-phenyl-2-pyrazoline. Melting point: 185°-187° C.

Aufarbeitung

  1. temperaturewas refluxed
  2. temperatureunder heating
  3. temperatureAfter cooling the mixture
  4. distillationthe solvent was distilled off under reduced pressure
  5. stirringthe residue was stirred together with ethyl ether
  6. customPrecipitated crystals
  7. filtrationwere collected by filtration
  8. washthoroughly washed with ethyl ether
  9. stirringthe suspension was stirred at room temperature for 5 minutes
  10. filtrationCrystals were collected by filtration
  11. washthoroughly washed with water
  12. dry with materialwith ethyl ether and dried

Quellen und Nachweise

ORD-Eintrag
ord-90aabf528e4f47538e659a6ed3c045f3
Quelldatensatz
uspto-grants-1994_10
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05354731

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