Potassium Carbonate → 2-(4-Aminophenylthio)benzoxazole

HRID 55082

Reaktionsgleichung

Reaktionsgleichung von HRID 55082
Cl[C:2]1[O:3][C:4]2[CH:10]=[CH:9][CH:8]=[CH:7][C:5]=2[N:6]=1.[NH2:11][C:12]1[CH:17]=[CH:16][C:15]([SH:18])=[CH:14][CH:13]=1.C(=O)([O-])[O-].[K+].[K+]>C(O)C>[NH2:11][C:12]1[CH:17]=[CH:16][C:15]([S:18][C:2]2[O:3][C:4]3[CH:10]=[CH:9][CH:8]=[CH:7][C:5]=3[N:6]=2)=[CH:14][CH:13]=1

Komponenten

5

Edukt 3

HCID 11430Potassium CarbonateHCID 119862-ChlorobenzoxazoleHCID 145104-Aminothiophenol

Produkt 1

HCID 137183792-(4-Aminophenylthio)benzoxazoleAusbeute 79,4 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

2-Chlorobenzoxazole (0.065 moles, 10.0 g), 4-aminothiophenol (0.065 moles, 8.1 g) and potassium carbonate (0.065 moles, 9.0 g) were stirred for 3 days at room temperature in 250 ml ethanol, filtered, and concentrated. Ethyl acetate was added and the solution washed with water, dried over sodium sulfate and concentrated. The product was purified by HPLC over silica gel eluted with 50% ethyl acetate in hexane to yield 2-(4-aminophenylthio)benzoxazole 12.5 g, 79%. Mass spec (FD) 243. Calculated for C11H10N2OS: C, 64.44; H, 4.16; N, 11.56. Found: C, 64.53; H, 4.22; N, 11.58.

Aufarbeitung

  1. filtrationfiltered
  2. concentrationconcentrated
  3. additionEthyl acetate was added
  4. washthe solution washed with water
  5. dry with materialdried over sodium sulfate
  6. concentrationconcentrated
  7. customThe product was purified by HPLC over silica gel
  8. washeluted with 50% ethyl acetate in hexane

Quellen und Nachweise

ORD-Eintrag
ord-5860be73be6247f7800a3889e6f128be
Quelldatensatz
uspto-grants-1997_04
Patentnummer
US05624937

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