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Sodium methanesulfonate → HCID 22747447、化合物

HRID 2246314
ノート
印刷プレビュー

反応式

HRID 2246314 の反応式
[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4](I)[C:3]=1[F:9].[CH3:10][S:11]([O-])(=[O:13])=[O:12].[Na+]>CN(C)C(=O)C.[Cu](I)I>[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([S:11]([CH3:10])(=[O:13])=[O:12])[C:3]=1[F:9]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 638112Sodium methanesulfonateHCID 190666581,2-Difluoro-3-iodobenzene

生成物 1

HCID 22747447HCID 22747447、化合物収率 72.5%

試薬・触媒・溶媒 2

HCID 83717Copper iodide触媒HCID 31374Dimethylacetamide溶媒

実験手順

1,2-Difluoro-3-iodobenzene (1.70 g; 7.08 mmol), 2.17 g (21.2 mmol) of sodium methanesulfonate and 4.03 g (21.2 mmol) of copper iodide were heated with stirring at 111° C. for 20 hours in 50 ml of N,N-dimethylacetamide. The reaction solution was filtered, chloroform was added to the filtrate and the mixture was washed with a saturated aqueous solution of sodium hydrogen carbonate. The organic layer was dried and concentrated and the resulting residue was purified by a silica gel column chromatography (hexane:ethyl acetate=2:1) to give 987 mg (yield: 72%) of 1,2-difluoro-3-methanesulfonylbenzene as a colorless transparent solution.

このページの内容参加物実験手順後処理出典と根拠反応ノート

後処理

  1. filtrationThe reaction solution was filtered
  2. additionchloroform was added to the filtrate
  3. washthe mixture was washed with a saturated aqueous solution of sodium hydrogen carbonate
  4. customThe organic layer was dried
  5. concentrationconcentrated
  6. customthe resulting residue was purified by a silica gel column chromatography (hexane:ethyl acetate=2:1)

出典と根拠

ORDレコード
ord-5ebaa3e9af374c4c97da47c985b54541
出典データセット
uspto-grants-2010_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07687502B2

反応ノート

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