Dimethylformamide → 1,3-Dichloro-2-fluoro-5-nitrobenzene

HRID 1709691

反応式

HRID 1709691 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([N+:10]([O-:12])=[O:11])[CH:5]=[C:6]([Cl:9])[C:7]=1Cl.[F-:13].[K+].CN(C)C=O>O>[Cl:1][C:2]1[CH:3]=[C:4]([N+:10]([O-:12])=[O:11])[CH:5]=[C:6]([Cl:9])[C:7]=1[F:13]

参加物

5

反応物 3

HCID 6228DimethylformamideHCID 883653,4,5-TrichloronitrobenzeneHCID 522689Potassium Fluoride2 回

生成物 1

HCID 765541,3-Dichloro-2-fluoro-5-nitrobenzene

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A mixture of 3,4,5-trichloronitrobenzene (13.55 g, 59 mmol), potassium fluoride (4.65 g, 80 mmol) and dimethylformamide (DMF; 66 ml) is heated at 140° for 15 hours. An additional 2.5 g of potassium fluoride is added and the mixture is stirred an additional 15 hours at 140°. The reaction mixture is poured into water and extracted with ether. The combined organic layers are washed with water and with brine and filtered, and the solvent is removed to give a dark solid, which is purified by column chromatography to give 3,5-dichloro-4-fluoronitrobenzene, a yellow powder.

後処理

  1. temperatureis heated at 140° for 15 hours
  2. extractionextracted with ether
  3. washThe combined organic layers are washed with water and with brine
  4. filtrationfiltered
  5. customthe solvent is removed
  6. customto give a dark solid, which
  7. customis purified by column chromatography

出典と根拠

ORDレコード
ord-3a22b09c30b14d1b975aac63b5bfbd61
出典データセット
uspto-grants-1990_08
特許番号
US04950678

関連ノート

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