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Sodium Iodide → Ethyl 2-(3-(trifluoromethyl)-1H-pyrazol-1-yl)acetate

HRID 1477598
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HRID 1477598 반응식
[F:1][C:2]([F:9])([F:8])[C:3]1[CH:7]=[CH:6][NH:5][N:4]=1.C(=O)([O-])[O-].[K+].[K+].Br[CH2:17][C:18]([O:20][CH2:21][CH3:22])=[O:19].[I-].[Na+].Cl.C(N=C=NCCCN(C)C)C.ON1C2C=CC=CC=2N=N1>C(Cl)(Cl)Cl.O.C(O)C>[F:1][C:2]([F:9])([F:8])[C:3]1[CH:7]=[CH:6][N:5]([CH2:17][C:18]([O:20][CH2:21][CH3:22])=[O:19])[N:4]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

10

반응물 6

HCID 5238Sodium IodideHCID 7748Ethyl bromoacetateHCID 11430Potassium CarbonateHCID 757711-HydroxybenzotriazoleHCID 18070343-(Trifluoromethyl)pyrazoleHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride

생성물 1

HCID 2064143
Ethyl 2-(3-(trifluoromethyl)-1H-pyrazol-1-yl)acetate

시약·촉매·용매 3

HCID 702Ethanol용매HCID 962Water용매HCID 6212Chloroform용매2회

실험 절차

To a chloroform solution (2 mL) of 3-(trifluoromethyl)-1H-pyrazole (68 mg, 0.50 mmol), potassium carbonate (104 mg, 0.75 mmol) and ethyl bromoacetate (100 mg, 0.60 mmol) were added and the resultant mixture was stirred at 70° C. for 2 hours. To the reaction solution, adequate amount of sodium iodide was added and the resultant mixture was further stirred for 1 day. To the reaction solution, 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (147 mg, 0.77 mmol), 1-hydroxybenzotriazole (catalytic amount) and ethanol (500 μL) were added and the resultant mixture was stirred for 2 hours. After completion of the reaction, water was added to the reaction solution and extraction with chloroform from the resultant mixture was performed. The organic layer was dried over anhydrous sodium sulfate and concentrated under reduced pressure to obtain a crude product of the title compound. The crude product was used in the next reaction as it was.

후처리

  1. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  2. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-c0ab7cc382e44ff9a758c647329e5b2b
출처 데이터셋
uspto-grants-2016_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09403798B2

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