Water → alpha,alpha-Bis(4-chlorophenyl)-1H-pyrazole-4-methanol

HRID 64634Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 64634
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]([C:16]2[CH:21]=[CH:20][C:19]([Cl:22])=[CH:18][CH:17]=2)([C:10]2[CH:11]=[N:12]C=[N:14][CH:15]=2)[OH:9])=[CH:4][CH:3]=1.NN.O>C(O)C>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]([C:16]2[CH:21]=[CH:20][C:19]([Cl:22])=[CH:18][CH:17]=2)([C:10]2[CH:11]=[N:12][NH:14][CH:15]=2)[OH:9])=[CH:4][CH:3]=1

Komponenten

5

Versuchsvorschrift

The methiodide salt of α,α-bis(4-chlorophenyl)-pyrimidine-5-methanol (12.8 g) was heated to reflux with 3 g of anhydrous hydrazine in ethanol. The original slurry went into solution and then a precipitate formed, at which time 25 ml of water were added. The mixture was heated at reflux for 20 minutes, filtered hot, water was added and the mixture was extracted with ether. The ether was evaporated and the residue was crystallized from chloroform to provide the title product, m.p. 135°-137° C. The NMR and mass spectra were consistent with the desired structure.

Aufarbeitung

  1. additionwere added
  2. temperatureThe mixture was heated
  3. temperatureat reflux for 20 minutes
  4. filtrationfiltered hot
  5. additionwater was added
  6. extractionthe mixture was extracted with ether
  7. customThe ether was evaporated
  8. customthe residue was crystallized from chloroform

Quellen und Nachweise

ORD-Eintrag
ord-883462650c1c42c3bb7da08a9468e273
Quelldatensatz
uspto-grants-1986_09
Patentnummer
US04609666

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