Acetic Acid → 63166-90-5

反応式

[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

参加物

反応物 4

HCID 176Acetic Acid

HCID 784Hydrogen Peroxide

HCID 962Water

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

生成物 1

HCID 1234629763166-90-5

実験手順

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.

後処理

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)

出典と根拠

ORDレコード: ord-587778ccf4c24ad690e7493d8eea9adf
出典データセット: uspto-grants-2013_10
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US08551993B2

反応ノート

読み込み中…

参加物