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

HRID 1993934
ノート
印刷プレビュー

反応式

HRID 1993934 の反応式
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
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

反応条件

温度
100 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-cfd31f0d0b53475ebca71ebc6a349a6d
出典データセット
uspto-grants-2010_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07652057B2

反応ノート

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