Tin tetrachloride → 4-(2,5-Dichlorophenoxy)-3-fluoroaniline

HRID 1993818

反応式

HRID 1993818 の反応式
[Cl:1][C:2]1[CH:18]=[CH:17][C:16]([Cl:19])=[CH:15][C:3]=1[O:4][C:5]1[CH:10]=[CH:9][C:8]([N+:11]([O-])=O)=[CH:7][C:6]=1[F:14].[Sn](Cl)(Cl)(Cl)Cl.C(=O)(O)[O-].[Na+]>C(O)C>[Cl:1][C:2]1[CH:18]=[CH:17][C:16]([Cl:19])=[CH:15][C:3]=1[O:4][C:5]1[CH:10]=[CH:9][C:8]([NH2:11])=[CH:7][C:6]=1[F:14]

参加物

5

反応物 3

HCID 24287Tin tetrachlorideHCID 516892Sodium BicarbonateHCID 597980461-(2,5-Dichloro-phenoxy)-2-fluoro-4-nitro-benzene

生成物 1

HCID 289727064-(2,5-Dichlorophenoxy)-3-fluoroaniline

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
70 °C

実験手順

A mixture of 1-(2,5-dichloro-phenoxy)-2-fluoro-4-nitro-benzene (0.5 g, 1.7 mmol) and tin chloride (1.57 g, 8.3 mmol) in 30 ml of anhydrous ethanol was heated to 70° C. under argon and stirred for 4 hours. The solution was allowed to cool and then poured into ice. The solution was made slightly basic (pH 7-8) by addition of saturated aqueous sodium bicarbonate solution, then extracted with ethyl acetate. The organic phase was thoroughly washed with brine and dried treated with anhydrous sodium sulfate. Evaporation of the solvent left a yellow oily product which was used for the next step without further purification.

後処理

  1. temperatureto cool
  2. additionpoured into ice
  3. extractionextracted with ethyl acetate
  4. washThe organic phase was thoroughly washed with brine
  5. customdried
  6. additiontreated with anhydrous sodium sulfate
  7. customEvaporation of the solvent
  8. waitleft a yellow oily product which
  9. customwas used for the next step without further purification

出典と根拠

ORDレコード
ord-088607fcf1674831b4d0ede632494377
出典データセット
uspto-grants-2010_01
特許番号
US07652047B2

関連ノート

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