Hydrochloric Acid → 3-Ethyl-4-oxo-4-(2-phenyl-benzoxazol-6-yl)-butyric acid

HRID 1619945Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1619945
C[Si]([N-][Si](C)(C)C)(C)C.[K+].[C:11]1([C:17]2[O:18][C:19]3[CH:25]=[C:24]([C:26](=[O:30])[CH2:27][CH2:28][CH3:29])[CH:23]=[CH:22][C:20]=3[N:21]=2)[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1.C[O:32][C:33](=[O:36])[CH2:34]Br.Cl>C1(C)C=CC=CC=1.C1COCC1>[CH2:28]([CH:27]([C:26](=[O:30])[C:24]1[CH:23]=[CH:22][C:20]2[N:21]=[C:17]([C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=3)[O:18][C:19]=2[CH:25]=1)[CH2:34][C:33]([OH:36])=[O:32])[CH3:29]

Komponenten

7

Reaktionsbedingungen

Temperatur
-78 °C

Versuchsvorschrift

625.00 μl (313 μmol) potassium bis(trimethylsilyl)amide 0.5M in toluene are placed in 15 ml THF and cooled to −78° C. 75.00 mg (283 μmol) 1-(2-phenyl-benzoxazol-6-yl)-butan-1-one, dissolved in 15 ml THF, are added dropwise to this solution and the mixture is stirred for 15 min at −78° C. Then 55 mg (360 μmol) methylbromoacetate, dissolved in 5 ml THF, are also added dropwise and the mixture is stirred for 30 min at −78° C., then 1N hydrochloric acid is added and the mixture is extracted with diethyl ether. The org. phase is dried on magnesium sulphate and the solv. is eliminated i.V.

Aufarbeitung

  1. additionare added dropwise to this solution
  2. additionare also added dropwise
  3. stirringthe mixture is stirred for 30 min at −78° C.
  4. extractionthe mixture is extracted with diethyl ether
  5. customphase is dried on magnesium sulphate

Quellen und Nachweise

ORD-Eintrag
ord-e10417453f1d4371aa095ac680b78911
Quelldatensatz
uspto-grants-2014_07
Patentnummer
US08772323B2

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