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

HRID 1086327
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반응식

HRID 1086327 반응식
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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-12c893f0a5424d7dafa1d8143455f13e
출처 데이터셋
uspto-grants-1991_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05028728

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