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Potassium Carbonate → ethyl 1-{2-[(3-fluorophenyl)amino]-2-oxoethyl}-4-nitro-1H-pyrazole-3-carboxylate

HRID 639974
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HRID 639974 반응식
[N+:1]([C:4]1[C:5]([C:9]([O:11][CH2:12][CH3:13])=[O:10])=[N:6][NH:7][CH:8]=1)([O-:3])=[O:2].Cl[CH2:15][C:16]([NH:18][C:19]1[CH:24]=[CH:23][CH:22]=[C:21]([F:25])[CH:20]=1)=[O:17].C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O>[F:25][C:21]1[CH:20]=[C:19]([NH:18][C:16](=[O:17])[CH2:15][N:7]2[CH:8]=[C:4]([N+:1]([O-:3])=[O:2])[C:5]([C:9]([O:11][CH2:12][CH3:13])=[O:10])=[N:6]2)[CH:24]=[CH:23][CH:22]=1
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참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 23889312-chloro-N-(3-fluorophenyl)acetamideHCID 178470496HCID 178470496, 화합물

생성물 1

HCID 68638240ethyl 1-{2-[(3-fluorophenyl)amino]-2-oxoethyl}-4-nitro-1H-pyrazole-3-carboxylate수율 74%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A mixture of ethyl 4-nitro-1H-pyrazole-3-carboxylate (0.685 g, 3.7 mmol) and 2-chloro-N-(3-fluorophenyl) acetamide (0.694 g, 3.7 mmol) and potassium carbonate (0.613 g, 4.44 mmol) in dimethyl formamide (10 ml) was stirred at room temperature for 20 hours. The mixture was evaporated and the residue was purified by silica gel chromatography eluting with a 8 to 10% mixture of ethyl acetate in dichloromethane to give ethyl 1-{2-[(3-fluorophenyl)amino]-2-oxoethyl}-4-nitro-1H-pyrazole-3-carboxylate (0.920 g, 74% yield):

후처리

  1. customThe mixture was evaporated
  2. customthe residue was purified by silica gel chromatography
  3. washeluting with a 8 to 10% mixture of ethyl acetate in dichloromethane

출처 및 근거

ORD 기록
ord-0c7ce77ca11f4c6f82d9997a73c036cd
출처 데이터셋
uspto-grants-2010_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07691867B2

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