Chlorosulfonic acid → 4-Methoxy-3-(trifluoromethyl)benzenesulfonyl chloride

HRID 2181870노트

반응식

HRID 2181870 반응식
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[C:9]([F:12])([F:11])[F:10].[Cl:13][S:14](O)(=[O:16])=[O:15]>C(Cl)(Cl)Cl>[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([S:14]([Cl:13])(=[O:16])=[O:15])=[CH:5][C:4]=1[C:9]([F:10])([F:11])[F:12]

참가 물질

4

반응물 2

HCID 24638Chlorosulfonic acidHCID 27752511-Methoxy-2-(trifluoromethyl)benzene

생성물 1

HCID 224823844-Methoxy-3-(trifluoromethyl)benzenesulfonyl chloride수율 56.2%

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

A solution of 1-methoxy-2-(trifluoromethyl)benzene (10.0 g, 56.8 mmol) in dry chloroform (76 mL) was cooled to 0° C. and treated with chlorosulfonic acid (7.55 mL, 113.5 mmol) drop-wise under argon. After the addition was completed, the reaction mixture was gradually warmed to room temperature and stirred overnight. The reaction was quenched by pouring the mixture slowly onto ice. The separated, aqueous phase was extracted with chloroform (3×). The combined organic phase was washed sequentially with a saturated, aqueous sodium chloride solution (2×) and water. The organic phase was dried over anhydrous magnesium sulfate and concentrated in vacuo to yield the title compound (8.77 g. 31.9 mmol, 56%) as a gray solid;

후처리

  1. additionAfter the addition
  2. customThe reaction was quenched
  3. additionby pouring the mixture slowly onto ice
  4. extractionThe separated, aqueous phase was extracted with chloroform (3×)
  5. washThe combined organic phase was washed sequentially with a saturated, aqueous sodium chloride solution (2×) and water
  6. dry with materialThe organic phase was dried over anhydrous magnesium sulfate
  7. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-454d07b0abb14def93e86a2a0fecf95b
출처 데이터셋
uspto-grants-2005_05
특허 번호
US06894061B2

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