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Ethyl 2-(ethoxymethylene)-4,4,4-trifluoroacetoacetate → ethyl 1-(4-cyanophenyl)-5-(trifluoromethyl)-1H-pyrazole-4-carboxylate

HRID 1799438
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HRID 1799438 반응식
C(O/[CH:4]=[C:5](/[C:11](=O)[C:12]([F:15])([F:14])[F:13])\[C:6]([O:8][CH2:9][CH3:10])=[O:7])C.Cl.[NH:18]([C:20]1[CH:27]=[CH:26][C:23]([C:24]#[N:25])=[CH:22][CH:21]=1)[NH2:19]>C(O)C>[C:24]([C:23]1[CH:26]=[CH:27][C:20]([N:18]2[C:11]([C:12]([F:13])([F:14])[F:15])=[C:5]([C:6]([O:8][CH2:9][CH3:10])=[O:7])[CH:4]=[N:19]2)=[CH:21][CH:22]=1)#[N:25]
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참가 물질

4

반응물 2

HCID 2737179Ethyl 2-(ethoxymethylene)-4,4,4-trifluoroacetoacetateHCID 162129624-Cyanophenylhydrazine Hydrochloride

생성물 1

HCID 59516077ethyl 1-(4-cyanophenyl)-5-(trifluoromethyl)-1H-pyrazole-4-carboxylate수율 77.4%

시약·촉매·용매 1

HCID 702Ethanol용매2회

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온도
-10 °C

실험 절차

A solution of (Z)-ethyl 2-(ethoxymethylene)-4,4,4-trifluoro-3-oxobutanoate (2.41 g, 10.03 mmol) in ethanol (10 mL) was added dropwise to a stirred solution of 4-hydrazinylbenzonitrile hydrochloride (1.702 g, 10.03 mmol), in ethanol (50 mL) cooled to −10° C. The resulting solution was allowed to stir at room temperature for 16 hours. The reaction mixture was evaporated to dryness and the residue redissolved in EtOAc (100 mL), and washed sequentially with water (50 mL) and saturated brine (50 mL). The organic layer was dried over MgSO4, filtered and evaporated to afford crude product. The crude product was purified by flash silica (120 g) chromatography, elution gradient 10 to 60% EtOAc in isohexane. Pure fractions were evaporated to dryness to afford ethyl 1-(4-cyanophenyl)-5-(trifluoromethyl)-1H-pyrazole-4-carboxylate (2.400 g, 77%) as a white solid.

후처리

  1. customThe reaction mixture was evaporated to dryness
  2. dissolutionthe residue redissolved in EtOAc (100 mL)
  3. washwashed sequentially with water (50 mL) and saturated brine (50 mL)
  4. dry with materialThe organic layer was dried over MgSO4
  5. filtrationfiltered
  6. customevaporated
  7. customto afford crude product
  8. customThe crude product was purified by flash silica (120 g) chromatography, elution gradient 10 to 60% EtOAc in isohexane
  9. customPure fractions were evaporated to dryness

출처 및 근거

ORD 기록
ord-f119780c47f848afaa6168558d712634
출처 데이터셋
uspto-grants-2013_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08344016B2

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