Chlorosulfonic acid → 5-fluoro-4-hydroxy-2-methylbenzenesulfonyl Chloride

HRID 243614ノート

反応式

HRID 243614 の反応式
[Cl:1][S:2]([OH:5])(=O)=[O:3].[F:6][C:7]1[CH:12]=[CH:11][C:10]([CH3:13])=[CH:9][C:8]=1[OH:14]>ClCCl>[F:6][C:7]1[C:8]([OH:14])=[CH:9][C:10]([CH3:13])=[C:11]([S:2]([Cl:1])(=[O:5])=[O:3])[CH:12]=1

参加物

4

反応物 2

HCID 24638Chlorosulfonic acidHCID 182387Phenol, 2-fluoro-5-methyl-

生成物 1

HCID 847898185-fluoro-4-hydroxy-2-methylbenzenesulfonyl Chloride収率 7.5%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of chlorosulfonic acid (1.5 g, 13.3 mmol) dissolved in 10 mL of dichloromethane was added 2-fluoro-5-methylphenol (1.1 g, 8.86 mmol) dropwise. After 10 minutes, the reaction was quenched by adding to ice water. The reaction was extracted with dichloromethane, washed with brine, dried over MgSO4, filtered, and concentrated to give 150 mg (7.5%) of the title compound.

後処理

  1. customthe reaction was quenched
  2. additionby adding to ice water
  3. extractionThe reaction was extracted with dichloromethane
  4. washwashed with brine
  5. dry with materialdried over MgSO4
  6. filtrationfiltered
  7. concentrationconcentrated

出典と根拠

ORDレコード
ord-9712bed19a3b48b08e5d273d585b8cf2
出典データセット
uspto-grants-2014_02
特許番号
US08653141B2

反応ノート

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