Pentamethylbenzene → Pentamethylbenzenesulphonyl chloride

HRID 1164283

反応式

HRID 1164283 の反応式
[CH3:1][C:2]1[C:3]([CH3:11])=[C:4]([CH3:10])[C:5]([CH3:9])=[C:6]([CH3:8])[CH:7]=1.[Cl:12][S:13](O)(=[O:15])=[O:14]>ClCCl>[CH3:8][C:6]1[C:7]([S:13]([Cl:12])(=[O:15])=[O:14])=[C:2]([CH3:1])[C:3]([CH3:11])=[C:4]([CH3:10])[C:5]=1[CH3:9]

参加物

4

反応物 2

HCID 12784PentamethylbenzeneHCID 24638Chlorosulfonic acid

生成物 1

HCID 590180Pentamethylbenzenesulphonyl chloride

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

In 500 ml of dichloromethane was dissolved 17.8 g of pentamethylbenzene and the solution was cooled to -5°~-10° C. A solution of 24 ml of chlorosulfonic acid in 400 ml of dichloromethane was added dropwise, and the mixture was allowed to stand at room temperature. The reaction mixture was poured into ice-5% aqueous sodium hydrogen carbonate. The organic layer was washed with water and dried over magnesium sulfate. Removal of the solvent by distillation leaves crystals which were collected by filtration and recrystallized from n-hexane. Yield 27.7 g (93.5%), m.p. 80°-81° C.

後処理

  1. temperaturethe solution was cooled to -5°~-10° C
  2. customto stand at room temperature
  3. washThe organic layer was washed with water
  4. dry with materialdried over magnesium sulfate
  5. customRemoval of the solvent
  6. distillationby distillation
  7. customleaves crystals which
  8. filtrationwere collected by filtration
  9. customrecrystallized from n-hexane

出典と根拠

ORDレコード
ord-9efd88accc034523963633bc445a77b8
出典データセット
uspto-grants-1983_01
特許番号
US04368150

関連ノート

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