Methanesulfonyl chloride → N-[2-bromo-5-(trifluoromethyl)phenyl]methanesulfonamide

HRID 505671

反応式

HRID 505671 の反応式
[Br:1][C:2]1[CH:8]=[CH:7][C:6]([C:9]([F:12])([F:11])[F:10])=[CH:5][C:3]=1[NH2:4].[CH3:13][S:14](Cl)(=[O:16])=[O:15]>N1C=CC=CC=1>[Br:1][C:2]1[CH:8]=[CH:7][C:6]([C:9]([F:10])([F:11])[F:12])=[CH:5][C:3]=1[NH:4][S:14]([CH3:13])(=[O:16])=[O:15]

参加物

4

反応物 2

HCID 31297Methanesulfonyl chlorideHCID 679892-Bromo-5-(trifluoromethyl)benzenamine

生成物 1

HCID 59430904N-[2-bromo-5-(trifluoromethyl)phenyl]methanesulfonamide収率 52%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

To a solution of 2-bromo-5-trifluoromethylaniline (3.18 g, 13.25 mmol) in pyridine (18 ml) was added methanesulfonyl chloride (1.03 ml, 13.25 mmol) and the mixture was stirred for 6 hours at room temperature. The solvent was removed in vacuo and the residue was diluted with chloroform. The organic layer was washed with water, 1N hydrochloric acid, a saturated sodium hydrogen carbonate solution and saturated brine and dried over anhydrous sodium sulfate. The solvent was removed in vacuo and the residue was purified by recrystallization to give the subject compound (2.18 g, 52%).

後処理

  1. customThe solvent was removed in vacuo
  2. additionthe residue was diluted with chloroform
  3. washThe organic layer was washed with water, 1N hydrochloric acid
  4. dry with materiala saturated sodium hydrogen carbonate solution and saturated brine and dried over anhydrous sodium sulfate
  5. customThe solvent was removed in vacuo
  6. customthe residue was purified by recrystallization

出典と根拠

ORDレコード
ord-5888ddb31d474185be9e29694440c5d9
出典データセット
uspto-grants-2010_08
特許番号
US07781479B2

関連ノート

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