4-Nitrobenzenesulfonyl chloride → 5-Chloro-2'-fluoro-2-[(4-nitrophenylsulfonyl)amino]benzophenone

HRID 374626

反応式

HRID 374626 の反応式
[NH2:1][C:2]1[CH:16]=[CH:15][C:14]([Cl:17])=[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].[N+:18]([C:21]1[CH:26]=[CH:25][C:24]([S:27](Cl)(=[O:29])=[O:28])=[CH:23][CH:22]=1)([O-:20])=[O:19]>N1C=CC=CC=1>[Cl:17][C:14]1[CH:15]=[CH:16][C:2]([NH:1][S:27]([C:24]2[CH:23]=[CH:22][C:21]([N+:18]([O-:20])=[O:19])=[CH:26][CH:25]=2)(=[O:28])=[O:29])=[C:3]([CH:13]=1)[C:4]([C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=1[F:12])=[O:5]

参加物

4

反応物 2

HCID 74044-Nitrobenzenesulfonyl chlorideHCID 699122-Amino-5-chloro-2'-fluorobenzophenone

生成物 1

HCID 104106845-Chloro-2'-fluoro-2-[(4-nitrophenylsulfonyl)amino]benzophenone

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

A mixture containing 24.9 g of 2-amino-5-chloro-2'-fluorobenzophenone and 22.1 g of 4-nitrophenylsulfonyl chloride is refluxed for 10 hours in pyridine. It is evaporated to dryness, water and ethyl acetate are then added and the ethyl acetate phase is washed with water and an aqueous solution of sodium chloride, dried over magnesium sulfate and evaporated under vacuum. The expected product precipitates on evaporation; it is filtered off and recrystallized from a DCM/isopropyl ether mixture to give 20 g.

後処理

  1. customIt is evaporated to dryness, water and ethyl acetate
  2. additionare then added
  3. washthe ethyl acetate phase is washed with water
  4. dry with materialan aqueous solution of sodium chloride, dried over magnesium sulfate
  5. customevaporated under vacuum
  6. customThe expected product precipitates on evaporation
  7. filtrationit is filtered off
  8. customrecrystallized from a DCM/isopropyl ether mixture
  9. customto give 20 g

出典と根拠

ORDレコード
ord-f5a10398d4ce4cd58693002033b11ffc
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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