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Water → 2-(2-Hydroxyethylthio)-4,5-bis-(p-methoxyphenyl)-thiazole

HRID 544659
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 544659
[Na].[CH3:2][O:3][C:4]1[CH:9]=[CH:8][C:7]([C:10]2[CH:14]([C:15]3[CH:20]=[CH:19][C:18]([O:21][CH3:22])=[CH:17][CH:16]=3)[S:13][C:12](=[S:23])[N:11]=2)=[CH:6][CH:5]=1.[CH2:24]1[O:26][CH2:25]1.O>C(O)C.C(Cl)Cl>[OH:26][CH2:25][CH2:24][S:23][C:12]1[S:13][C:14]([C:15]2[CH:20]=[CH:19][C:18]([O:21][CH3:22])=[CH:17][CH:16]=2)=[C:10]([C:7]2[CH:8]=[CH:9][C:4]([O:3][CH3:2])=[CH:5][CH:6]=2)[N:11]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 4

HCID 962WaterHCID 6354Ethylene Oxide2×HCID 5360545SodiumHCID 132096564,5-Bis-(p-methoxyphenyl)-thiazoline-2-thione

Produkt 1

HCID 132096672-(2-Hydroxyethylthio)-4,5-bis-(p-methoxyphenyl)-thiazole

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 702
Ethanol
Lösungsmittel
HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

0.23 g of sodium are dissolved in 30 ml of ethanol under nitrogen. The solution is allowed to cool to room temperature, while stirring 3 g of 4,5-bis-(p-methoxyphenyl)-thiazoline-2-thione are added and, once dissolution is complete, ethylene oxide is introduced, the reaction temperature being maintained at 25°-30° by gentle cooling. After introducing the ethylene oxide for 30 minutes, it should not be possible to detect any more thione by thin layer chromatography. 10 ml of 2 N-ammonium chloride are then added, the ethanol is removed by distillation under reduced pressure, and the residue obtained by concentration by evaporation is shaken with a mixture of 50 ml of water and 50 ml of methylene chloride. The organic phase is removed, then shaken with methylene chloride, dried over magnesium sulphate and concentrated to dryness by evaporation. The oily crude product is caused to crystallise by triturating with 20 ml of diethyl ether and dried under reduced pressure. 2-(2-Hydroxyethylthio)-4,5-bis-(p-methoxyphenyl)-thiazole having a melting point of 82°-83° is obtained.

Aufarbeitung

  1. additionare added
  2. dissolutiononce dissolution
  3. temperaturethe reaction temperature being maintained at 25°-30° by gentle cooling
  4. customthe ethanol is removed by distillation under reduced pressure
  5. customthe residue obtained by concentration by evaporation
  6. customThe organic phase is removed
  7. dry with materialdried over magnesium sulphate
  8. concentrationconcentrated to dryness by evaporation
  9. customto crystallise
  10. customby triturating with 20 ml of diethyl ether
  11. customdried under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-62e166691814466c81d0b0a1dee02f90
Quelldatensatz
uspto-grants-1984_05
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04451471

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