Acetic Acid → 63166-90-5

Reaktionsgleichung

[Br:1][C:2]1[CH:11]=[CH:10][C:5]2[S:6][C:7]([CH3:9])=[CH:8][C:4]=2[CH:3]=1.OO.[OH2:14].C(O)(=[O:17])C>>[Br:1][C:2]1[CH:11]=[CH:10][C:5]2[S:6](=[O:17])(=[O:14])[C:7]([CH3:9])=[CH:8][C:4]=2[CH:3]=1

Komponenten

Edukt 4

HCID 176Acetic Acid

HCID 784Hydrogen Peroxide

HCID 962Water

HCID 136630355-Bromo-2-methyl-1-benzothiophene

Produkt 1

HCID 1234629763166-90-5

Versuchsvorschrift

5-Bromo-2-methylbenzo[b]thiophene (8.0 g, 35.2 mmol; prepared according to J. Med. Chem. 1986, 29, 1643) was dissolved in acetic acid (200 mL); 30% hydrogen peroxide (50 mL) was added and the mixture was refluxed for 4 h. Water (500 mL) was added and the mixture was extracted with benzene (300 mL). The organic layer was evaporated in vacuo and the residue was purified by column chromatography (silica gel Fluka 60, benzene) affording 5-bromo-2-methylbenzo[b]thiophene-1,1-dioxide.

Aufarbeitung

temperaturethe mixture was refluxed for 4 h
extractionthe mixture was extracted with benzene (300 mL)
customThe organic layer was evaporated in vacuo
customthe residue was purified by column chromatography (silica gel Fluka 60, benzene)

Quellen und Nachweise

ORD-Eintrag: ord-f2e175698df6473ba764c1d5ae9143ad
Quelldatensatz: uspto-grants-2011_05
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US07943613B2

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