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Hydrazine hydrate (1:1) → 3-cyclopropyl-4,5-dihydro-1H-pyrazol-5-one

HRID 1993934
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HRID 1993934 반응식
C[O:2][C:3](=O)[CH2:4][C:5]([CH:7]1[CH2:9][CH2:8]1)=O.O.[NH2:12][NH2:13]>C(O)(=O)C>[CH:7]1([C:5]2[CH2:4][C:3](=[O:2])[NH:12][N:13]=2)[CH2:9][CH2:8]1
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참가 물질

4

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 101300163-Cyclopropyl-3-Oxopropionic Acid Methyl Ester

생성물 1

HCID 220594943-cyclopropyl-4,5-dihydro-1H-pyrazol-5-one수율 147%

시약·촉매·용매 1

HCID 176Acetic Acid용매

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온도
100 °C

실험 절차

To a solution of methyl-3-cyclopropyl-3-oxopropionate (10 g) and acetic acid (28 mL) in a round bottom flask under argon was added hydrazine hydrate (2.25 g). The mixture was immersed into an oil bath and heated to 100° C. overnight. The reaction vessel was then cooled and the acetic acid was evaporated in vacuo and the remaining solid was added to 1 N aqueous sodium hydroxide solution. The resulting precipitate was collected by filtration and washed with water and cold ether to afford the desired 5-cyclopropyl-2,4-dihydro-pyrazol-3-one (8.2 g) as a beige solid.

후처리

  1. customThe mixture was immersed into an oil bath
  2. temperatureThe reaction vessel was then cooled
  3. customthe acetic acid was evaporated in vacuo
  4. additionthe remaining solid was added to 1 N aqueous sodium hydroxide solution
  5. filtrationThe resulting precipitate was collected by filtration
  6. washwashed with water and cold ether

출처 및 근거

ORD 기록
ord-cfd31f0d0b53475ebca71ebc6a349a6d
출처 데이터셋
uspto-grants-2010_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07652057B2

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