Hydrochloric Acid → 4-fluoro-1-(propan-2-yl)-1H-pyrazole-5-carboxylic acid

HRID 244657ノート

反応式

HRID 244657 の反応式
[F:1][C:2]1[CH:3]=[N:4][N:5]([CH:12]([CH3:14])[CH3:13])[C:6]=1[C:7]([O:9]CC)=[O:8].Cl>O1CCOCC1>[F:1][C:2]1[CH:3]=[N:4][N:5]([CH:12]([CH3:14])[CH3:13])[C:6]=1[C:7]([OH:9])=[O:8]

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 58356353ethyl 4-fluoro-1-(1-methylethyl)-1H-pyrazole-5-carboxylate

生成物 1

HCID 583563414-fluoro-1-(propan-2-yl)-1H-pyrazole-5-carboxylic acid収率 23.3%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

To a solution of ethyl 4-fluoro-1-(1-methylethyl)-1H-pyrazole-5-carboxylate (100 mg) in 1,4-dioxane (2 ml) was added 2M hydrochloric acid (2 ml) and the mixture heated at reflux under nitrogen for 58 h, allowed to stand at room temperature for 62 h, then heated at reflux under Nitrogen for 72 h. The mixture was cooled to room temperature and the solvent was removed in vacuo. Toluene (15 ml) was added and the solvent removed in vacuo to give a white solid that was dried in a vacuum oven overnight to give the title compound (20 mg) as a white solid.

後処理

  1. temperaturethe mixture heated
  2. temperatureat reflux under nitrogen for 58 h
  3. temperatureheated
  4. temperatureat reflux under Nitrogen for 72 h
  5. customthe solvent was removed in vacuo
  6. additionToluene (15 ml) was added
  7. customthe solvent removed in vacuo
  8. customto give a white solid
  9. customthat was dried in a vacuum oven overnight

出典と根拠

ORDレコード
ord-6f6d183073d742b2b56c8012a9678987
出典データセット
uspto-grants-2014_02
特許番号
US08658635B2

反応ノート

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