Acetic Acid → 2-[4,5-Bis-(p-methoxyphenyl)-thiazol-2-ylthio]-acetaldehyde

HRID 544655Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 544655
C[O:2][CH:3](OC)[CH2:4][S:5][C:6]1[S:7][C:8]([C:19]2[CH:24]=[CH:23][C:22]([O:25][CH3:26])=[CH:21][CH:20]=2)=[C:9]([C:11]2[CH:16]=[CH:15][C:14]([O:17][CH3:18])=[CH:13][CH:12]=2)[N:10]=1.C(O)(=O)C.S(=O)(=O)(O)O.O>C(OCC)(=O)C>[CH3:18][O:17][C:14]1[CH:15]=[CH:16][C:11]([C:9]2[N:10]=[C:6]([S:5][CH2:4][CH:3]=[O:2])[S:7][C:8]=2[C:19]2[CH:24]=[CH:23][C:22]([O:25][CH3:26])=[CH:21][CH:20]=2)=[CH:12][CH:13]=1

Komponenten

6

Edukt 4

HCID 176Acetic AcidHCID 962WaterHCID 1118Sulfuric AcidHCID 132096712-[4,5-Bis-(p-methoxyphenyl)-thiazol-2-ylthio]-acetaldehyde-dimethylacetal

Produkt 1

HCID 132096722-[4,5-Bis-(p-methoxyphenyl)-thiazol-2-ylthio]-acetaldehyde

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8857Ethyl AcetateLösungsmittel2×

Versuchsvorschrift

7.0 g of 2-[4,5-bis-(p-methoxyphenyl)-thiazol-2-ylthio]-acetaldehyde-dimethylacetal are mixed with 50 ml of acetic acid, 25 ml of sulphuric acid and 25 ml of water, stirred vigorously for 30 minutes, and then stirred into 1000 ml of ice-water. The oil which separates is taken up in 200 ml of ethyl acetate. Shaking is carried out with a further 200 ml of ethyl acetate and the combined organic phases are washed with water and then twice with cold sodium bicarbonate solution, dried over magnesium sulphate and concentrated to dryness by evaporation. The crude product is crystallised with diethyl ether. 2-[4,5-bis-(p-methoxyphenyl)-thiazol-2-ylthio]-acetaldehyde having a melting point of 75°-76° is obtained.

Aufarbeitung

  1. stirringShaking
  2. washthe combined organic phases are washed with water
  3. dry with materialtwice with cold sodium bicarbonate solution, dried over magnesium sulphate
  4. concentrationconcentrated to dryness by evaporation
  5. customThe crude product is crystallised with diethyl ether

Quellen und Nachweise

ORD-Eintrag
ord-dd213e223f904ea895d9f60ffebc329f
Quelldatensatz
uspto-grants-1984_05
Patentnummer
US04451471

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