Potassium Hydroxide → 1-Ethyl-3-trifluoromethyl-1H-pyrazole-4-carboxylic acid

HRID 374419ノート

反応式

HRID 374419 の反応式
[CH2:1]([N:3]1[CH:7]=[C:6]([C:8]([O:10]CC)=[O:9])[C:5]([C:13]([F:16])([F:15])[F:14])=[N:4]1)[CH3:2].[OH-].[K+]>C(O)C.O>[CH2:1]([N:3]1[CH:7]=[C:6]([C:8]([OH:10])=[O:9])[C:5]([C:13]([F:15])([F:14])[F:16])=[N:4]1)[CH3:2]

参加物

5

反応物 2

HCID 14797Potassium HydroxideHCID 18996914Ethyl 1-ethyl-3-(trifluoromethyl)-1H-pyrazole-4-carboxylate

生成物 1

HCID 189969211-Ethyl-3-trifluoromethyl-1H-pyrazole-4-carboxylic acid収率 97.3%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

Ethyl 1-ethyl-3-trifluoromethylpyrazole-4-carboxylate (2.17 g) was dissolved in ethanol and potassium hydroxide (1.06 g) in water was added. The reaction was stirred at room temperature overnight. Ethanol was removed under reduced pressure and the resulting residue partitioned between water and ether. The aqueous layer was separated, acidified with hydrochloric acid (2M) and extracted with ether. The combined organic extracts were dried over anhydrous magnesium sulphate and evaporated in vacuo to give 1-ethyl-3-trifluoromethylpyrazole-4-carboxylic acid as a white solid (1.86 g). NMR (CDCl3) δ1.45(t,3H), 4.20(q,2H), 7.95(s,1H).

後処理

  1. customEthanol was removed under reduced pressure
  2. customthe resulting residue partitioned between water and ether
  3. customThe aqueous layer was separated
  4. extractionextracted with ether
  5. dry with materialThe combined organic extracts were dried over anhydrous magnesium sulphate
  6. customevaporated in vacuo

出典と根拠

ORDレコード
ord-af4729e6010847c8ab096931b504e87a
出典データセット
uspto-grants-1996_01
特許番号
US05480857

反応ノート

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