Chlorosulfonic acid → 5-(2,6-Dichloro-4-trifluoromethylphenyl)-2-methylbenzenesulfonyl chloride

HRID 1432759노트

반응식

HRID 1432759 반응식
[Cl:1][C:2]1[CH:7]=[C:6]([C:8]([F:11])([F:10])[F:9])[CH:5]=[C:4]([Cl:12])[C:3]=1[C:13]1[CH:18]=[CH:17][C:16]([CH3:19])=[CH:15][CH:14]=1.[Cl:20][S:21](O)(=[O:23])=[O:22]>C(Cl)(Cl)Cl>[Cl:1][C:2]1[CH:7]=[C:6]([C:8]([F:9])([F:10])[F:11])[CH:5]=[C:4]([Cl:12])[C:3]=1[C:13]1[CH:18]=[CH:17][C:16]([CH3:19])=[C:15]([S:21]([Cl:20])(=[O:23])=[O:22])[CH:14]=1

참가 물질

4

반응물 2

HCID 24638Chlorosulfonic acidHCID 221709614-(2,6-Dichloro-4-trifluoromethylphenyl)toluene

생성물 1

HCID 221709435-(2,6-Dichloro-4-trifluoromethylphenyl)-2-methylbenzenesulfonyl chloride수율 81.1%

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

6.7 g (22.0 mmol) of 4-(2,6-dichloro-4-trifluoromethylphenyl)toluene prepared in (a) was dissolved in 50 ml of chloroform, and 3.8 g (32.6 mmol) of chlorosulfonic acid was added dropwise at 0° C. with stirring. After further 3 hours of stirring at room temperature, the reaction mixture was poured into about 200 ml of ice-cold water for separation. The organic layer was washed with water twice and dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure to obtain 7.2 g of 5-(2,6-dichloro-4-trifluoromethylphenyl)-2-methylbenzenesulfonyl chloride (yield 81.0%).

후처리

  1. stirringAfter further 3 hours of stirring at room temperature
  2. washThe organic layer was washed with water twice
  3. dry with materialdried over anhydrous magnesium sulfate
  4. distillationThe solvent was distilled off under reduced pressure

출처 및 근거

ORD 기록
ord-d457bb89c25148788266a891bf666d0c
출처 데이터셋
uspto-grants-2009_11
특허 번호
US07612105B2

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