Acetic Anhydride → Acetic acid, 2-(4-methylphenyl)hydrazide

HRID 906476

반응식

HRID 906476 반응식
Cl.[CH3:2][C:3]1[CH:8]=[CH:7][C:6]([NH:9][NH2:10])=[CH:5][CH:4]=1.C(=O)([O-])[O-].[K+].[K+].[C:17](OC(=O)C)(=[O:19])[CH3:18]>C(OC(C)C)(=O)C.O>[CH3:2][C:3]1[CH:8]=[CH:7][C:6]([NH:9][NH:10][C:17](=[O:19])[CH3:18])=[CH:5][CH:4]=1

참가 물질

6

반응물 3

HCID 7918Acetic AnhydrideHCID 11430Potassium CarbonateHCID 125044-Methylphenylhydrazine monohydrochloride

생성물 1

HCID 539992Acetic acid, 2-(4-methylphenyl)hydrazide

시약·촉매·용매 2

HCID 962Water용매HCID 7915Isopropyl Acetate용매

반응 조건

온도
57.5 °C

실험 절차

104.8 g of 1-(4-methylphenyl)hydrazine hydrochloride are suspended in 525 ml of isopropyl acetate, a solution of 104.8 g of potassium carbonate in 300 ml of water is added and then the mixture is stirred until the solid has disappeared. 77.4 g of acetic anhydride are added while maintaining the temperature below 20° C. and then the mixture is left stirring at 20° C. A precipitate is observed to form, which precipitate disappears when the mixture is heated at approximately 55-60° C. The organic phase is washed twice with 200 ml of water and is then cooled at 0-5° C. overnight. The product formed is recovered by filtration and is then washed twice with 100 ml of MTBE.

후처리

  1. temperaturewhile maintaining the temperature below 20° C.
  2. waitthe mixture is left
  3. stirringstirring at 20° C
  4. customto form
  5. customwhich precipitate
  6. washThe organic phase is washed twice with 200 ml of water
  7. temperatureis then cooled at 0-5° C. overnight
  8. customThe product formed
  9. filtrationis recovered by filtration
  10. washis then washed twice with 100 ml of MTBE

출처 및 근거

ORD 기록
ord-1e65d96aedb34060af22115503bdac19
출처 데이터셋
uspto-grants-2011_09
특허 번호
US08012991B2

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