Chlorosulfonic acid → 2-Methoxy-5-(2-oxopropyl)benzenesulfonyl chloride

HRID 34433

反応式

HRID 34433 の反応式
[Cl:1][S:2]([OH:5])(=O)=[O:3].[CH3:6][O:7][C:8]1[CH:13]=[CH:12][C:11]([CH2:14][C:15](=[O:17])[CH3:16])=[CH:10][CH:9]=1>>[Cl:1][S:2]([C:13]1[CH:12]=[C:11]([CH2:14][C:15](=[O:17])[CH3:16])[CH:10]=[CH:9][C:8]=1[O:7][CH3:6])(=[O:5])=[O:3]

参加物

3

反応物 2

HCID 24638Chlorosulfonic acidHCID 312311-(p-Methoxyphenyl)-2-propanone

生成物 1

HCID 131062582-Methoxy-5-(2-oxopropyl)benzenesulfonyl chloride収率 40%

実験手順

To 250 g of chlorosulfonic acid was added dropwise 50 g of 4-methoxyphenylacetone at 0°-5° C. After stirring the mixture for 4 hours at room temperature, the reaction mixture was poured into 2,500 ml of ice water and extracted thrice with 500 ml of ethyl acetate. The extract was washed with water and after drying the extract with anhydrous magnesium sulfate, the solvent was distilled off under reduced pressure. The crude crystals obtained were recrystallized from benzeneether to provide 32 g of 3-chlorosulfonyl-4-methoxyphenylacetone.

後処理

  1. extractionextracted thrice with 500 ml of ethyl acetate
  2. washThe extract was washed with water
  3. customafter drying the
  4. extractionextract with anhydrous magnesium sulfate
  5. distillationthe solvent was distilled off under reduced pressure
  6. customThe crude crystals obtained
  7. customwere recrystallized from benzeneether

出典と根拠

ORDレコード
ord-0d2c11c9a0654cc6a1af8168abb1e68e
出典データセット
uspto-grants-1988_08
特許番号
US04761500

関連ノート

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