Mci-186 → 1-Phenyl-3-methyl-4-formyl-5-pyrazolone

HRID 382796

Reaktionsgleichung

Reaktionsgleichung von HRID 382796
[CH3:1][C:2]1[CH2:6][C:5](=[O:7])[N:4]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[N:3]=1.P(Cl)(Cl)(Cl)=O.CN(C)[CH:21]=[O:22]>>[CH3:1][C:2]1[CH:6]([CH:21]=[O:22])[C:5](=[O:7])[N:4]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[N:3]=1

Komponenten

4

Edukt 3

HCID 4021Mci-186HCID 6228DimethylformamideHCID 24813Phosphorus oxychloride

Produkt 1

HCID 2051061-Phenyl-3-methyl-4-formyl-5-pyrazoloneAusbeute 65 %

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

29 Grams of 3-methyl-1-phenyl-2-pyrazoline-5-one and 40 ml of dimethylformamide were charged into a 200-ml three-necked flask, stirred and cooled to 0° C. in an ice-acetone bath. Then, 18.5 g of phosphorus oxychloride (POCl3) was placed in a dropping funnel, and while it was maintained at 10 to 20° C., it was dropwise added. After the addition, the mixture was heated for 1 hour, then, a reaction mixture was poured into 600 ml of ice water, and the mixture was allowed to stand for one day and night. A crystal was recovered by suction filtration, fully washed with water and dried to give the captioned compound. Yield: 65%, Melting point: 178-180° C. (documented value: 174-175° C.).

Aufarbeitung

  1. temperaturewhile it was maintained at 10 to 20° C.
  2. additionit was dropwise added
  3. additionAfter the addition
  4. temperaturethe mixture was heated for 1 hour
  5. filtrationA crystal was recovered by suction filtration
  6. washfully washed with water
  7. customdried
  8. customto give the captioned compound
  9. customYield: 65%, Melting point: 178-180° C. (documented value: 174-175° C.)

Quellen und Nachweise

ORD-Eintrag
ord-d6ce87e9240240ba9fb72e807c70bda7
Quelldatensatz
uspto-grants-2001_10
Patentnummer
US06310215B1

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