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Aniline → 2,2-Bis-(4-anilino-3-nitrophenyl)-hexafluoropropane

HRID 1086327
ノート
印刷プレビュー

反応式

HRID 1086327 の反応式
S(O[C:6]1[CH:11]=[CH:10][C:9]([C:12]([C:21]2[CH:26]=[CH:25][C:24](OS(C)(=O)=O)=[C:23]([N+:32]([O-:34])=[O:33])[CH:22]=2)([C:17]([F:20])([F:19])[F:18])[C:13]([F:16])([F:15])[F:14])=[CH:8][C:7]=1[N+:35]([O-:37])=[O:36])(C)(=O)=O.[NH2:38][C:39]1[CH:44]=[CH:43][CH:42]=[CH:41][CH:40]=1>C(#N)C>[NH:38]([C:6]1[CH:11]=[CH:10][C:9]([C:12]([C:21]2[CH:26]=[CH:25][C:24]([NH:32][C:23]3[CH:24]=[CH:25][CH:26]=[CH:21][CH:22]=3)=[C:23]([N+:32]([O-:34])=[O:33])[CH:22]=2)([C:17]([F:20])([F:19])[F:18])[C:13]([F:16])([F:15])[F:14])=[CH:8][C:7]=1[N+:35]([O-:37])=[O:36])[C:39]1[CH:44]=[CH:43][CH:42]=[CH:41][CH:40]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 6115AnilineHCID 142050422,2-Bis-(4-mesyloxy-3-nitrophenyl)-hexafluoropropane

生成物 1

HCID 142050452,2-Bis-(4-anilino-3-nitrophenyl)-hexafluoropropane収率 159.3%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

A solution of 60 g (0.103 mol) of 2,2-bis-(4-mesyloxy-3-nitrophenyl)-hexafluoropropane and 122.8 g (1.32 mol) of aniline in 400 ml of acetonitrile is heated under reflux for 24 hours. In the course of this the methanesulfonic acid salt of aniline is precipitated, and is removed by filtration with suction. The filtrate is freed from the solvent and from excess aniline by distillation under reduced pressure. Recrystallizing the residue from ethanol gives 47.3 g of 2,2-bis-(4-anilino-3-nitrophenyl)-hexafluoropropane (80% yield). M.p. 165-166° C.

後処理

  1. temperatureunder reflux for 24 hours
  2. customIn the course of this the methanesulfonic acid salt of aniline is precipitated
  3. customis removed by filtration with suction
  4. distillationThe filtrate is freed from the solvent and from excess aniline by distillation under reduced pressure
  5. customRecrystallizing the residue from ethanol

出典と根拠

ORDレコード
ord-12c893f0a5424d7dafa1d8143455f13e
出典データセット
uspto-grants-1991_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05028728

反応ノート

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