4-Aminophenol → 2-p-Tolylbenzoxazole

HRID 1414172

Reaktionsgleichung

Reaktionsgleichung von HRID 1414172
[CH3:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]([OH:10])=O)=[CH:6][CH:7]=1.[CH:11]1[C:16]([NH2:17])=[CH:15][CH:14]=[C:13](O)[CH:12]=1.B(O)(O)O>O>[C:2]1([CH3:1])[CH:7]=[CH:6][C:5]([C:8]2[O:10][C:15]3[CH:14]=[CH:13][CH:12]=[CH:11][C:16]=3[N:17]=2)=[CH:4][CH:3]=1

Komponenten

5

Edukt 3

HCID 4034-AminophenolHCID 7470P-Toluic AcidHCID 7628Boric Acid2×

Produkt 1

HCID 700392-p-Tolylbenzoxazole

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel2×

Versuchsvorschrift

68 g (0.5 mole of p-toluic acid were heated with 54.5 g (0.5 mole) of p-aminophenol and 2 g of boric acid in 750 ml of 1,2-methylnaphthalene and the water that formed was eliminated slowly by azeotropic destillation. After heating for 6 hours, 1 g of boric acid were added. After 12 hours, 16 ml of H2O (98%) passed over. The solvent was then removed until dryness, the residue was dissolved in 750 ml of ethanol, clarified with silica gel while still hot, and combined after filtration, while still hot, with 500 ml of H2O. After cooling and filtration with suction at room temperature and washing with aqueous ethanol, there were obtained 89.4 g (85.6% of the theory) of 2-p-tolyl-benzoxazole melting at 113° to 114° C. ##STR41##

Aufarbeitung

  1. temperatureAfter heating for 6 hours
  2. customThe solvent was then removed until dryness
  3. dissolutionthe residue was dissolved in 750 ml of ethanol
  4. filtrationafter filtration
  5. temperatureAfter cooling
  6. filtrationfiltration with suction at room temperature
  7. washwashing with aqueous ethanol

Quellen und Nachweise

ORD-Eintrag
ord-0bd8dd6b36004a5ba9e1e51078d19f80
Quelldatensatz
uspto-grants-1977_01
Patentnummer
US04001221

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