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

HRID 606521
ノート
印刷プレビュー

反応式

HRID 606521 の反応式
[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
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

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒
このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート

反応条件

温度
80 °C

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-6de0b517e36f403b8d8c09f3adb76c16
出典データセット
uspto-grants-2011_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07915267B2

反応ノート

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