Ethanol → 3-Bromo-5-fluoro-2-iodoaniline

HRID 1078429

反応式

HRID 1078429 の反応式
[I:1][C:2]1[C:7]([Br:8])=[CH:6][C:5]([F:9])=[CH:4][C:3]=1[N+:10]([O-])=O.O.O.[Sn](Cl)Cl.C(O)C.C(=O)([O-])O.[Na+]>C(OCC)(=O)C>[I:1][C:2]1[C:7]([Br:8])=[CH:6][C:5]([F:9])=[CH:4][C:3]=1[NH2:10]

参加物

6

反応物 4

HCID 702EthanolHCID 61436Stannous chloride dihydrateHCID 516892Sodium BicarbonateHCID 194297701-Bromo-5-fluoro-2-iodo-3-nitrobenzene

生成物 1

HCID 194297943-Bromo-5-fluoro-2-iodoaniline収率 76%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

Treat 1-iodo-2-nitro-4-fluoro-6-bromobenzene (5.0 g, 14.46 mmol) with tin (II) chloride dihydrate (12 g, 58 mmol) in refluxing ethanol (150 mL). Stir at reflux for 24 hours, pour into a mixture of ethyl acetate (200 mL) and saturated sodium hydrogen carbonate (500 mL). Filter and wash the filtrate with saturated sodium hydrogen carbonate (200 mL) and water (200 mL). Dry (MgSO4), evaporate the solvent in vacuo and purify by silica gel chromatography to give the title compound as an off-white solid (3.45 g, 76%).

後処理

  1. temperatureat reflux for 24 hours
  2. filtrationFilter
  3. washwash the filtrate with saturated sodium hydrogen carbonate (200 mL) and water (200 mL)
  4. dry with materialDry (MgSO4)
  5. customevaporate the solvent in vacuo
  6. custompurify by silica gel chromatography

出典と根拠

ORDレコード
ord-612d69fd98c442d1b8b9c0e0315fa898
出典データセット
uspto-grants-1996_08
特許番号
US05547991

関連ノート

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