Calcium hypochlorite → 5-Propionyl-3-phenylisoxazole

HRID 345178

Reaktionsgleichung

Reaktionsgleichung von HRID 345178
[OH:1][CH:2]([C:5]1[O:9][N:8]=[C:7]([C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)[CH:6]=1)[CH2:3][CH3:4].Cl.N1C=CC=CC=1.Cl[O-].[Ca+2].Cl[O-]>ClCCl>[C:2]([C:5]1[O:9][N:8]=[C:7]([C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)[CH:6]=1)(=[O:1])[CH2:3][CH3:4]

Komponenten

5

Edukt 3

HCID 24504Calcium hypochloriteHCID 10176127Pyridinium chlorideHCID 151807655-(1-Hydroxypropyl)-3-phenylisoxazole

Produkt 1

HCID 151807665-Propionyl-3-phenylisoxazole

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

In 10 ml of dichloromethane, 1.0 g (5.0 mmol) of 5-(1-hydroxypropyl)-3-phenylisoxazole was dissolved. To the solution were added 100 mg (0.9 mmol) of pyridine hydrochloride, followed by the further addition of 1.4 g (9.9 mmol) of calcium hypochlorite. They were reacted at room temperature for 5 hours. After completion of the reaction, insoluble matter was filtered off and the organic layer was washed with water. The organic layer was dried over anhydrous sodium sulfate and the solvent was distilled off under reduced pressure. The residue was then recrystallized from ethanol, whereby the target compound, namely, 5-propionyl-3-phenylisoxazole was obtained as crystals.

Aufarbeitung

  1. customThey were reacted at room temperature for 5 hours
  2. customAfter completion of the reaction, insoluble matter
  3. filtrationwas filtered off
  4. washthe organic layer was washed with water
  5. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  6. distillationthe solvent was distilled off under reduced pressure
  7. customThe residue was then recrystallized from ethanol, whereby the target compound

Quellen und Nachweise

ORD-Eintrag
ord-eb37384716134ff39c15317a1454392c
Quelldatensatz
uspto-grants-1991_10
Patentnummer
US05055585

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