Sulfuric Acid → HCID 13537597, Verbindung

HRID 638550Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 638550
[C:1]([C:9]1[CH:13]=[C:12]([CH2:14][CH2:15][OH:16])[O:11][N:10]=1)(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[OH:17]S(O)(=O)=O>C(Cl)Cl.S([O-])(O)(=O)=O.C([N+](CCCC)(CCCC)CCCC)CCC>[C:1]([C:9]1[CH:13]=[C:12]([CH2:14][C:15]([OH:17])=[O:16])[O:11][N:10]=1)(=[O:8])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

Komponenten

5

Edukt 2

HCID 1118Sulfuric AcidHCID 13809953[5-(2-Hydroxyethyl)-1,2-oxazol-3-yl](phenyl)methanone

Produkt 1

HCID 13537597HCID 13537597, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 94433Tetrabutylammonium hydrogen sulfateKatalysatorHCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

To a mixture of 8.8 g of 2-(3-benzoylisoxazol-5-yl)ethanol, in 1 liter of CH2Cl2, a few crystals of tetra-n-butylammonium hydrogen sulfate and 150 ml of 9M H2SO4 was added 11.9 g (41 mmol) of pulverized K2Cr2O7. The resulting mixture was stirred at room temperature for 1.5 hour. After allowing the mixture to settle, it was decanted from the unreacted dichromate. The aqueous phase was extracted with CH2Cl2, and the organics were washed with water and brine, and dried over MgSO4. Concentration gave a wet solid which was triturated with cyclohexane and collected to give 7.1 g of a solid. Recrystallization from toluene gave 4.0 g (43%) of a solid, m.p. 108°-110°.

Aufarbeitung

  1. customit was decanted from the unreacted dichromate
  2. extractionThe aqueous phase was extracted with CH2Cl2
  3. washthe organics were washed with water and brine
  4. dry with materialdried over MgSO4
  5. concentrationConcentration
  6. customgave a wet solid which
  7. customwas triturated with cyclohexane
  8. customcollected

Quellen und Nachweise

ORD-Eintrag
ord-d1747f17d061448a86aa676a7fff1ee8
Quelldatensatz
uspto-grants-1985_12
Patentnummer
US04562187

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