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

HRID 374419노트

반응식

HRID 374419 반응식
[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]

참가 물질

5

반응물 2

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

생성물 1

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

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-af4729e6010847c8ab096931b504e87a
출처 데이터셋
uspto-grants-1996_01
특허 번호
US05480857

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