4-Toluenesulfonyl chloride → N-(2-(o-Fluorobenzoyl)-4-nitrophenyl)-p-toluenesulphonamide

HRID 374628

反応式

HRID 374628 の反応式
[NH2:1][C:2]1[CH:16]=[CH:15][C:14]([N+:17]([O-:19])=[O:18])=[CH:13][C:3]=1[C:4]([C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=1[F:12])=[O:5].[S:20](Cl)([C:23]1[CH:29]=[CH:28][C:26]([CH3:27])=[CH:25][CH:24]=1)(=[O:22])=[O:21]>N1C=CC=CC=1>[F:12][C:7]1[CH:8]=[CH:9][CH:10]=[CH:11][C:6]=1[C:4](=[O:5])[C:3]1[CH:13]=[C:14]([N+:17]([O-:19])=[O:18])[CH:15]=[CH:16][C:2]=1[NH:1][S:20]([C:23]1[CH:29]=[CH:28][C:26]([CH3:27])=[CH:25][CH:24]=1)(=[O:22])=[O:21]

参加物

4

反応物 2

HCID 73974-Toluenesulfonyl chlorideHCID 676572-Amino-2'-fluoro-5-nitrobenzophenone

生成物 1

HCID 3023542N-(2-(o-Fluorobenzoyl)-4-nitrophenyl)-p-toluenesulphonamide

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

A mixture containing 10 g of 2-amino-5-nitro-2'-fluorobenzophenone and 7.5 g of tosyl chloride is refluxed in 50 ml of pyridine for 24 hours. The solvent is evaporated off to dryness, water and ethyl acetate are added, an insoluble material is filtered off and the organic phase is washed with a dilute solution of hydrochloric acid, water and an aqueous solution of sodium chloride and then dried over magnesium sulfate and evaporated. The residue is chromatographed on silica and the expected product is eluted with DCM.

後処理

  1. customThe solvent is evaporated off to dryness, water and ethyl acetate
  2. additionare added
  3. filtrationan insoluble material is filtered off
  4. washthe organic phase is washed with a dilute solution of hydrochloric acid, water
  5. dry with materialan aqueous solution of sodium chloride and then dried over magnesium sulfate
  6. customevaporated
  7. customThe residue is chromatographed on silica
  8. washthe expected product is eluted with DCM

出典と根拠

ORDレコード
ord-3cd3151d66c7437c86a3b83b45c13a04
出典データセット
uspto-grants-1996_01
特許番号
US05481005

関連ノート

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