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Water → 4-(Methylsulfonyl)-3-(trifluoromethyl)aniline

HRID 2086687
ノート
印刷プレビュー

反応式

HRID 2086687 の反応式
[CH3:1][S:2]([C:5]1[CH:10]=[CH:9][C:8]([N+:11]([O-])=O)=[CH:7][C:6]=1[C:14]([F:17])([F:16])[F:15])(=[O:4])=[O:3].[Cl-].[NH4+].O>C(O)C.[Fe]>[CH3:1][S:2]([C:5]1[CH:10]=[CH:9][C:8]([NH2:11])=[CH:7][C:6]=1[C:14]([F:15])([F:16])[F:17])(=[O:4])=[O:3]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 962WaterHCID 25517Ammonium ChlorideHCID 206051531-(Methylsulphonyl)-4-nitro-2-(trifluoromethyl)benzene

生成物 1

HCID 223166824-(Methylsulfonyl)-3-(trifluoromethyl)aniline収率 76.2%

試薬・触媒・溶媒 2

HCID 23925Iron触媒HCID 702Ethanol溶媒

実験手順

A mixture of 4-(methylsulfonyl)-3-(trifluoromethyl)nitrobenzene (1.55 g, 5.76 mmol), iron powder (1.61 g, 28.8 mmol), and ammonium chloride (0.031 g, 0.58 mmol) in ethanol (30 mL), and water (8 mL) was heated at reflux temperature for 1 hour. After cooling, insolubles were filtered off by Celite, and volatiles were removed by evaporation. The residue was redissolved in ethyl acetate (50 mL) and the whole washed with water and brine. After dried over MgSO4 and concentration in vacuo. The residue was washed with hexane to give the subtitle compound (1.05 g, 76.2%, yield).

後処理

  1. temperaturewas heated
  2. temperatureat reflux temperature for 1 hour
  3. temperatureAfter cooling
  4. filtrationinsolubles were filtered off by Celite, and volatiles
  5. customwere removed by evaporation
  6. dissolutionThe residue was redissolved in ethyl acetate (50 mL)
  7. washthe whole washed with water and brine
  8. dry with materialAfter dried over MgSO4 and concentration in vacuo
  9. washThe residue was washed with hexane

出典と根拠

ORDレコード
ord-d6caa9f1beb44fac8d42da5688a16d86
出典データセット
uspto-grants-2004_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06727238B2

反応ノート

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