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Methanol → 2-(5-oxo-2,5-dihydro-1H-pyrazol-3-yl)acetic acid

HRID 606521
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HRID 606521 반응식
[O:1]=[C:2]1[NH:6][NH:5][C:4]([CH2:7][C:8]([O:10]CC)=[O:9])=[CH:3]1.CO.O.[OH-].[Na+]>C1COCC1>[O:1]=[C:2]1[NH:6][NH:5][C:4]([CH2:7][C:8]([OH:10])=[O:9])=[CH:3]1
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참가 물질

6

반응물 4

HCID 887MethanolHCID 962WaterHCID 14798Sodium HydroxideHCID 43831447ethyl (5-oxo-2,5-dihydro-1H-pyrazol-3-yl)acetate

생성물 1

HCID 167653152-(5-oxo-2,5-dihydro-1H-pyrazol-3-yl)acetic acid수율 82%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매
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반응 조건

온도
80 °C

실험 절차

To a suspension of ethyl (5-oxo-2,5-dihydro-1H-pyrazol-3-yl)acetate obtained in Reference Example 117 (5.00 g, 29.4 mmol) in THF (20 mL)-methanol (20 mL)-water (20 mL) was added 5N aqueous sodium hydroxide solution (11.0 mL, 88.0 mmol) at room temperature, and the mixture was stirred under heating at 80° C. for 3 hr. The reaction mixture allowed to cool to room temperature, and concentrated under reduced pressure, and the residue was diluted with water, and acidified with 6N hydrochloric acid. The precipitated solid was collected by filtration, and washed with water, and dried under nitrogen stream to give the title compound as a white powder (3.43 g, 82%).

후처리

  1. temperatureto cool to room temperature
  2. concentrationconcentrated under reduced pressure
  3. additionthe residue was diluted with water
  4. filtrationThe precipitated solid was collected by filtration
  5. washwashed with water
  6. customdried under nitrogen stream

출처 및 근거

ORD 기록
ord-6de0b517e36f403b8d8c09f3adb76c16
출처 데이터셋
uspto-grants-2011_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07915267B2

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