Sulfuric Acid → 2-(2,6-Difluorophenyl)acetohydrazide

HRID 727836

反応式

HRID 727836 の反応式
[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([F:8])[C:3]=1[CH2:9][C:10]([OH:12])=O.S(=O)(=O)(O)O.O.[NH2:19][NH2:20]>C(O)C>[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([F:8])[C:3]=1[CH2:9][C:10]([NH:19][NH2:20])=[O:12]

参加物

5

反応物 3

HCID 1118Sulfuric AcidHCID 24654Hydrazine hydrate (1:1)HCID 1235852,6-Difluorophenylacetic acid

生成物 1

HCID 199075982-(2,6-Difluorophenyl)acetohydrazide

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

70.4 g (0.41 mol) of 2,6-difluorophenylacetic acid, 700 ml of ethanol and 35 ml of concentrated sulphuric acid are heated under reflux for 3 hours. The reaction mixture is then concentrated by evaporation, taken up in dichloromethane and the solution is extracted by shaking in succession with water, 2N sodium carbonate solution and again with water. After drying over magnesium sulphate, the organic phase is concentrated by evaporation. The residue is dissolved in 560 ml of ethanol. After the addition of 30 ml (31 g; 0.62 mol) of hydrazine hydrate, the whole is heated under reflux for 4 days. After cooling, the resulting crystals are filtered off to yield 56.4 g (74% of the theoretical yield) of 2,6-difluorophenylacetic acid hydrazide which melts at 177°-178°.

後処理

  1. temperatureunder reflux for 3 hours
  2. concentrationThe reaction mixture is then concentrated by evaporation
  3. extractionthe solution is extracted
  4. dry with materialAfter drying over magnesium sulphate
  5. concentrationthe organic phase is concentrated by evaporation
  6. dissolutionThe residue is dissolved in 560 ml of ethanol
  7. temperaturethe whole is heated
  8. temperatureunder reflux for 4 days
  9. temperatureAfter cooling
  10. filtrationthe resulting crystals are filtered off
  11. customto yield 56.4 g (74% of the

出典と根拠

ORDレコード
ord-5775217f908247bcab4ceb1b16638d8e
出典データセット
uspto-grants-1991_09
特許番号
US05045556

関連ノート

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