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

HRID 34433

반응식

HRID 34433 반응식
[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]

참가 물질

3

반응물 2

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

생성물 1

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

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-0d2c11c9a0654cc6a1af8168abb1e68e
출처 데이터셋
uspto-grants-1988_08
특허 번호
US04761500

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