Acetic Acid → HCID 67067321, 화합물

HRID 599591노트

반응식

HRID 599591 반응식
C(O)(=O)C.[F:5][C:6]1[CH:11]=[CH:10][C:9]([CH:12]2[CH2:16][CH2:15][O:14][C:13]2=[O:17])=[CH:8][CH:7]=1.[NH2:18][NH2:19].N>CO.C(OCC)(=O)C>[F:5][C:6]1[CH:11]=[CH:10][C:9]([CH:12]([CH2:16][CH2:15][OH:14])[C:13]([NH:18][NH2:19])=[O:17])=[CH:8][CH:7]=1

참가 물질

7

반응물 4

HCID 176Acetic AcidHCID 222AmmoniaHCID 9321HydrazineHCID 22013226HCID 22013226, 화합물

생성물 1

HCID 67067321HCID 67067321, 화합물수율 31.8%

시약·촉매·용매 2

HCID 887Methanol용매HCID 8857Ethyl Acetate용매

실험 절차

Acetic acid (1 mL) was added to a solution of 3-(4-fluorophenyl)dihydrofuran-2-one (393 mg) and hydrazine (699 mg) in methanol (10 mL), and the reaction solution was heated to reflux for two hours. The reaction solution was left to cool to room temperature. Then, ethyl acetate and concentrated aqueous ammonia were added to the reaction solution, and the organic layer was separated. The resulting organic layer was dried over anhydrous magnesium sulfate and then concentrated under reduced pressure. Chloroform was added to the residue, and the precipitated solid was collected by filtration to obtain 147 mg of the title compound. The property values of the compound are as follows.

후처리

  1. temperaturethe reaction solution was heated
  2. temperatureto reflux for two hours
  3. waitThe reaction solution was left
  4. customthe organic layer was separated
  5. dry with materialThe resulting organic layer was dried over anhydrous magnesium sulfate
  6. concentrationconcentrated under reduced pressure
  7. additionChloroform was added to the residue
  8. filtrationthe precipitated solid was collected by filtration

출처 및 근거

ORD 기록
ord-b107cb6310c3429e805db945ccc07133
출처 데이터셋
uspto-grants-2011_03
특허 번호
US07897632B2

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