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

HRID 2181870ノート

反応式

HRID 2181870 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

HCID 224823844-Methoxy-3-(trifluoromethyl)benzenesulfonyl chloride収率 56.2%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

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;

後処理

  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

出典と根拠

ORDレコード
ord-454d07b0abb14def93e86a2a0fecf95b
出典データセット
uspto-grants-2005_05
特許番号
US06894061B2

反応ノート

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