Formic Acid → HCID 178471160, 화합물

HRID 349922노트

반응식

HRID 349922 반응식
C([N:8]1[C:12]([C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)=[C:11](/[CH:19]=[CH:20]/[C:21]([O:23][CH2:24][CH3:25])=[O:22])[CH:10]=[N:9]1)C1C=CC=CC=1.C(O)=O>[C].[Pd].C(O)C>[C:13]1([C:12]2[C:11]([CH2:19][CH2:20][C:21]([O:23][CH2:24][CH3:25])=[O:22])=[CH:10][NH:9][N:8]=2)[CH:14]=[CH:15][CH:16]=[CH:17][CH:18]=1

참가 물질

5

반응물 2

HCID 284Formic AcidHCID 69421709ethyl(E)-3-(1-benzyl-5-phenyl-1H-pyrazol-4-yl)propenoate

생성물 1

HCID 178471160HCID 178471160, 화합물수율 55%

시약·촉매·용매 2

HCID 178418390HCID 178418390, 화합물촉매HCID 702Ethanol용매

실험 절차

A mixture of ethyl(E)-3-(1-benzyl-5-phenyl-1H-pyrazol-4-yl)propenoate (300 mg), 5% palladium-carbon (600 mg), formic acid (3 ml), and ethanol (10 ml) was refluxed for 2 hours. After the palladium-carbon was removed by filtration, the filtrate was concentrated. The residue was dissolved in ethyl acetate, washed with saturated aqueous sodium bicarbonate and then with saturated aqueous sodium chloride solution, dried (MgSO4), and concentrated. The residue was subjected to silica gel column chromatography, and ethyl 3-(3-phenyl-1H-pyrazol-4-yl)propionate (120 mg, yield: 55%) was obtained as a colorless oily substance from the fraction eluted with ethyl acetate-hexane (2:3, volume ratio).

후처리

  1. temperaturewas refluxed for 2 hours
  2. customAfter the palladium-carbon was removed by filtration
  3. concentrationthe filtrate was concentrated
  4. dissolutionThe residue was dissolved in ethyl acetate
  5. washwashed with saturated aqueous sodium bicarbonate
  6. dry with materialwith saturated aqueous sodium chloride solution, dried (MgSO4)
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-683a847c3939419b9d3560a82b15c42f
출처 데이터셋
uspto-grants-2007_02
특허 번호
US07179823B1

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