Ethanol → Ethyl 1-ethyl-1H-pyrazole-5-carboxylate

HRID 244659

反応式

HRID 244659 の反応式
[CH2:1]([N:3]1[C:7]([C:8]([OH:10])=[O:9])=[CH:6][CH:5]=[N:4]1)[CH3:2].S(=O)(=O)(O)O.[CH2:16](O)[CH3:17]>>[CH2:1]([N:3]1[C:7]([C:8]([O:10][CH2:16][CH3:17])=[O:9])=[CH:6][CH:5]=[N:4]1)[CH3:2]

参加物

4

反応物 3

HCID 702EthanolHCID 1118Sulfuric AcidHCID 5657021-Ethyl-1H-pyrazole-5-carboxylic acid

生成物 1

HCID 23005846Ethyl 1-ethyl-1H-pyrazole-5-carboxylate

実験手順

To a solution of 1-ethyl-1H-pyrazole-5-carboxylic acid (950 mg) (for example, available from Fluorochem) in ethanol (50 ml) was added sulphuric acid (0.5 ml) and the mixture stirred at reflux under nitrogen for 70 h. The solvent was removed in vacuo and the residue partitioned between DCM (25 ml) and saturated sodium bicarbonate solution (25 ml) and separated using a hydrophobic frit. The aqueous layer was washed with DCM (2×20 ml) and the organic phases were combined. The solvent was removed in vacuo to give the title compound (1.09 g) as a colourless oil.

後処理

  1. temperatureat reflux under nitrogen for 70 h
  2. customThe solvent was removed in vacuo
  3. customthe residue partitioned between DCM (25 ml) and saturated sodium bicarbonate solution (25 ml)
  4. customseparated
  5. washThe aqueous layer was washed with DCM (2×20 ml)
  6. customThe solvent was removed in vacuo

出典と根拠

ORDレコード
ord-d52b561c3c0e42b09f4229878d584849
出典データセット
uspto-grants-2014_02
特許番号
US08658635B2

関連ノート

読み込み中…