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Pyridine → N-(4-bromo-2-fluoro-5-methylphenyl)methanesulfonamide

HRID 876128
ノート
印刷プレビュー

反応式

HRID 876128 の反応式
[Br:1][C:2]1[C:8]([CH3:9])=[CH:7][C:5]([NH2:6])=[C:4]([F:10])[CH:3]=1.N1C=CC=CC=1.[CH3:17][S:18](Cl)(=[O:20])=[O:19]>C(Cl)Cl>[Br:1][C:2]1[C:8]([CH3:9])=[CH:7][C:5]([NH:6][S:18]([CH3:17])(=[O:20])=[O:19])=[C:4]([F:10])[CH:3]=1
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 3

HCID 1049PyridineHCID 31297Methanesulfonyl chlorideHCID 70180404-Bromo-2-fluoro-5-methylaniline

生成物 1

HCID 67066531N-(4-bromo-2-fluoro-5-methylphenyl)methanesulfonamide収率 99.2%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of 4-bromo-2-fluoro-5-methylaniline (2.04 g, 10.0 mmol) in anhydrous CH2Cl2 (20 ml) and pyridine (3.23 ml, 40.0 mmol) was added methanesulfonyl chloride (0.86 ml, 11.0 mmol) and the resulting mixture was stirred at room temperature for 2 h. Solvent was removed in vacuo, and the residue was partitioned between EtOAc and 1M aq. HCl. The organic layer was washed with saturated aqueous NaHCO3, brine and then dried over Na2SO4. The drying agent was filtered off, and the filtrate was concentrated to give the title compound as a solid (2.80 g, 99%).

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. customSolvent was removed in vacuo
  2. customthe residue was partitioned between EtOAc and 1M aq. HCl
  3. washThe organic layer was washed with saturated aqueous NaHCO3, brine
  4. dry with materialdried over Na2SO4
  5. filtrationThe drying agent was filtered off
  6. concentrationthe filtrate was concentrated

出典と根拠

ORDレコード
ord-2850328cd2a14aebb4c42b784d9a12ed
出典データセット
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08986740B2

反応ノート

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