p-Toluenesulfonic acid → HCID 22252737, Verbindung

HRID 1278846Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1278846
[Br:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[S:8][CH2:9][CH:10]=[C:11]([CH3:13])[CH3:12].C1(C)C=CC(S(O)(=O)=O)=CC=1>C1(C)C=CC=CC=1>[CH3:12][C:11]1([CH3:13])[C:4]2[C:3](=[C:2]([Br:1])[CH:7]=[CH:6][CH:5]=2)[S:8][CH2:9][CH2:10]1

Komponenten

4

Edukt 2

HCID 6101p-Toluenesulfonic acidHCID 106348752-Bromo-1-(3-methylbut-2-enylthio)benzene

Produkt 1

HCID 22252737HCID 22252737, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel

Versuchsvorschrift

26.00 g (102.0 mmol) of 2-bromo-1-(3-methylbut-2-enylthio)benzene, 180 ml of toluene and 23.20 g (122.0 mmol) of para-toluenesulphonic acid are introduced into a three-necked flask. The reaction medium is refluxed for four hours and is then evaporated to dryness. The residue is taken up in aqueous sodium hydrogen carbonate solution and extracted with ethyl acetate, and the organic phase is separated out after settling, dried over magnesium sulphate and evaporated The residue obtained is purified by chromatography on a column of silica and eluted with heptane. 20 g (76%) of the expected compound are collected in the form of an orange-coloured oil.

Aufarbeitung

  1. temperatureThe reaction medium is refluxed for four hours
  2. customis then evaporated to dryness
  3. extractionextracted with ethyl acetate
  4. customthe organic phase is separated out
  5. dry with materialdried over magnesium sulphate
  6. customevaporated The residue
  7. customobtained
  8. customis purified by chromatography on a column of silica
  9. washeluted with heptane
  10. custom20 g (76%) of the expected compound are collected in the form of an orange-coloured oil

Quellen und Nachweise

ORD-Eintrag
ord-33282732a5ef4740abb05351ad4002b9
Quelldatensatz
uspto-grants-2002_09
Patentnummer
US06444709B1

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