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Hydrochloric Acid → 1-ethyl-4-fluoro-1H-pyrazole-5-carboxylic acid

HRID 244661
ノート
印刷プレビュー

反応式

HRID 244661 の反応式
[CH2:1]([N:3]1[C:7]([C:8]([O:10]CC)=[O:9])=[C:6]([F:13])[CH:5]=[N:4]1)[CH3:2].Cl>O1CCOCC1>[CH2:1]([N:3]1[C:7]([C:8]([OH:10])=[O:9])=[C:6]([F:13])[CH:5]=[N:4]1)[CH3:2]
参加物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 313Hydrochloric AcidHCID 58356399ethyl 1-ethyl-4-fluoro-1H-pyrazole-5-carboxylate

生成物 1

HCID 583564401-ethyl-4-fluoro-1H-pyrazole-5-carboxylic acid収率 45.7%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

To a solution of ethyl 1-ethyl-4-fluoro-1H-pyrazole-5-carboxylate (67 mg) in 1,4-dioxane (3 ml) was added 2M hydrochloric acid (2 ml) was added and the mixture was heated at reflux under nitrogen for 120 h. The mixture was cooled to room temperature and the solvent was removed in vacuo. Toluene (15 ml) was added and the solvent was removed in vacuo to give a solid that was dried in a vacuum oven overnight to give the title compound (26 mg) as a brown solid.

後処理

  1. additionwas added
  2. temperaturethe mixture was heated
  3. temperatureat reflux under nitrogen for 120 h
  4. customthe solvent was removed in vacuo
  5. additionToluene (15 ml) was added
  6. customthe solvent was removed in vacuo
  7. customto give a solid
  8. customthat was dried in a vacuum oven overnight

出典と根拠

ORDレコード
ord-11e4c56967834f96826b35e474adafa2
出典データセット
uspto-grants-2014_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08658635B2

反応ノート

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