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

HRID 1709691

반응식

HRID 1709691 반응식
[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]

참가 물질

5

반응물 3

HCID 6228DimethylformamideHCID 883653,4,5-TrichloronitrobenzeneHCID 522689Potassium Fluoride2회

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-3a22b09c30b14d1b975aac63b5bfbd61
출처 데이터셋
uspto-grants-1990_08
특허 번호
US04950678

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