Hydrochloric Acid → {2-[4-(Trifluoromethyl)phenyl]hydrazinylidene}acetic acid

HRID 859854

반응식

HRID 859854 반응식
[F:1][C:2]([F:12])([F:11])[C:3]1[CH:8]=[CH:7][C:6]([NH:9][NH2:10])=[CH:5][CH:4]=1.Cl.[C:14]([OH:18])(=[O:17])[CH:15]=O.C(OCC)(=O)C>O>[F:1][C:2]([F:11])([F:12])[C:3]1[CH:4]=[CH:5][C:6]([NH:9][N:10]=[CH:15][C:14]([OH:18])=[O:17])=[CH:7][CH:8]=1

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 760Glyoxylic AcidHCID 8857Ethyl AcetateHCID 1362004-(Trifluoromethyl)phenylhydrazine

생성물 1

HCID 69587423{2-[4-(Trifluoromethyl)phenyl]hydrazinylidene}acetic acid수율 88%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

4-Trifluoromethylphenyl hydrazine (4.1 g, 23 mmol) was gradually added to a solution of concentrated hydrochloric acid (5 ml) in water (120 ml). 40% aqueous solution (4.3 g, 23 mmol) of glyoxylic acid was gradually added, and stirred at room temperature for 5 hours. After leaving it overnight, the mixture was extracted with ethyl acetate. The organic phase was washed with a saturated brine, and dried on anhydrous sodium sulfate. The solvent was distilled off, and the resulting crystals were washed with hexane and a little amount of ethyl acetate to obtain (4-trifluoromethylphenyl hydrazono) acetic acid (4.7 g, 20 mmol, 88%).

후처리

  1. customAfter leaving it overnight
  2. extractionthe mixture was extracted with ethyl acetate
  3. washThe organic phase was washed with a saturated brine
  4. dry with materialdried on anhydrous sodium sulfate
  5. distillationThe solvent was distilled off
  6. washthe resulting crystals were washed with hexane

출처 및 근거

ORD 기록
ord-99c30590289d4d38ac20e226ef70e8f1
출처 데이터셋
uspto-grants-2006_12
특허 번호
US07153815B2

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