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Toluene → 1H-Pyrazole--toluene (1/1)

HRID 1472767
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1472767
[OH-].[Na+].[C:3]1([CH3:9])[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.C[NH:11][NH2:12]>O>[NH:11]1[CH:9]=[CH:3][CH:4]=[N:12]1.[C:3]1([CH3:9])[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 1140TolueneHCID 6061MethylhydrazineHCID 14798Sodium Hydroxide

Produkt 1

HCID 714149961H-Pyrazole--toluene (1/1)

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel2×

Reaktionsbedingungen

Temperatur
-10 °C

Versuchsvorschrift

A 2000-ml three-neck flask was equipped with a dropping funnel and a thermometer and sealed under a nitrogen balloon. Into this flask, 36.0 g of water, 6.4 g of sodium hydroxide, 400 ml of toluene and 24.0 g (0.52 mol) of monomethylhydrazine were placed. The resulting solution was cooled, with stirring, to −10° C. or lower in a low-temperature thermostat whose temperature was set to −15° C. Then, 375 g of the water-washed DFAAE-toluene solution (DFAAE: 0.11 mol) was gradually dropped into the flask through the dropping funnel in such a manner that the inside temperature of the flask did not exceed −10° C. After completion of the dropping, the solution was kept stirred for 1 hour at −12° C. The inside temperature of the flask was then raised to 0° C. The thus-obtained solution was separated with the addition of 400 ml of water. The organic phase was recovered by a separatory funnel and washed with 400 ml of water, thereby yielding 702 g of 9.7 mass % pyrazole-toluene solution.

Aufarbeitung

  1. customA 2000-ml three-neck flask was equipped with a dropping funnel
  2. customa thermometer and sealed under a nitrogen balloon
  3. temperatureThe resulting solution was cooled
  4. customwas set to −15° C
  5. additionwas gradually dropped into the flask through the dropping funnel in such a manner that the inside temperature of the flask
  6. customdid not exceed −10° C
  7. stirringAfter completion of the dropping, the solution was kept stirred for 1 hour at −12° C
  8. temperatureThe inside temperature of the flask was then raised to 0° C
  9. customThe thus-obtained solution was separated with the addition of 400 ml of water
  10. customThe organic phase was recovered by a separatory funnel
  11. washwashed with 400 ml of water

Quellen und Nachweise

ORD-Eintrag
ord-4e24e00ae14944889c97e6494f576a8f
Quelldatensatz
uspto-grants-2015_04
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US09012657B2

Notizen zur Reaktion

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