Ethyl Acetate → HCID 178418534, Verbindung

HRID 3781

Reaktionsgleichung

Reaktionsgleichung von HRID 3781
[O:1]([C:8]1[CH:13]=[CH:12][C:11]([OH:14])=[CH:10][CH:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[C:15](=O)([O-])[O-].[K+].[K+].BrC[C:23]1[S:24][C:25]([O:28][CH2:29][CH3:30])=[N:26][N:27]=1.C(OCC)(=O)C>CC(C)=O>[CH2:29]([O:28][C:25]1[SH:24]([CH3:15])[C:23]([O:14][C:11]2[CH:10]=[CH:9][C:8]([O:1][C:2]3[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=3)=[CH:13][CH:12]=2)=[N:27][N:26]=1)[CH3:30]

Komponenten

6

Edukt 4

HCID 8857Ethyl AcetateHCID 11430Potassium CarbonateHCID 132544-PhenoxyphenolHCID 201533922-Bromomethyl-5-ethoxy-1,3,4-thiadiazole

Produkt 1

HCID 178418534HCID 178418534, VerbindungAusbeute 74,2 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 180AcetoneLösungsmittel

Versuchsvorschrift

0.76 g of 4-phenoxy phenol was dissolved in 10 ml of acetone followed by adding 0.6 g of anhydrous potassium carbonate and 1.0 g of 2-bromomethyl-5-ethoxy-1,3,4-thiadiazole. The resulting mixture was refluxed with stirring and heated for 2 hours. After cooling, 100 ml of ethyl acetate was added followed by washing with water for two times, and the resulting ethyl acetate layer was dried over anhydrous magnesium sulfate. Ethyl acetate was distilled over under reduced pressure, and the residue was purified by chromatography on silica gel to obtain 1.0 g of the compound No. 1 described in Table 1.

Aufarbeitung

  1. temperatureThe resulting mixture was refluxed
  2. temperatureheated for 2 hours
  3. temperatureAfter cooling
  4. washby washing with water for two times
  5. dry with materialthe resulting ethyl acetate layer was dried over anhydrous magnesium sulfate
  6. distillationEthyl acetate was distilled over under reduced pressure
  7. customthe residue was purified by chromatography on silica gel

Quellen und Nachweise

ORD-Eintrag
ord-f72db97d8ce54dbba8cafdb5ed72d91d
Quelldatensatz
uspto-grants-1988_02
Patentnummer
US04722934

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