Water → 2-(1-(2-Fluoro-4-nitrophenyl)-3-pyrazolyl)pyridine

HRID 1844503

반응식

HRID 1844503 반응식
[NH:1]1[CH:5]=[CH:4][C:3]([C:6]2[CH:11]=[CH:10][CH:9]=[CH:8][N:7]=2)=[N:2]1.[F:12][C:13]1[CH:14]=[C:15]([N+:20]([O-:22])=[O:21])[CH:16]=[CH:17][C:18]=1F.C(=O)([O-])[O-].[K+].[K+].O>CN(C)C=O>[F:12][C:13]1[CH:14]=[C:15]([N+:20]([O-:22])=[O:21])[CH:16]=[CH:17][C:18]=1[N:1]1[CH:5]=[CH:4][C:3]([C:6]2[CH:11]=[CH:10][CH:9]=[CH:8][N:7]=2)=[N:2]1

참가 물질

6

반응물 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 1230531,2-Difluoro-4-nitrobenzeneHCID 27976572-(1H-Pyrazol-3-Yl)Pyridine

생성물 1

HCID 867193702-(1-(2-Fluoro-4-nitrophenyl)-3-pyrazolyl)pyridine수율 93.4%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

Compound 17a (1 g, 6.9 mmol) obtained from the aforesaid process and 3,4-difluoro-nitrobenzene (0.74 mL) were dissolved in N,N-dimethylformamide (20 mL), and then anhydrous potassium carbonate (1.9 g) was added thereto. The mixture was reacted at 100° C. for 4 hours. After completion of the reaction, the reactant mixture was cooled to room temperature. Water was added to the mixture, resulting in a substantial amount of precipitate. Then, the precipitate was suction-filtered, and the filter cake was recrystallized with acetone to get the product 18a as a white powder (1.7 g), with a yield of 93.4%.

후처리

  1. customThe mixture was reacted at 100° C. for 4 hours
  2. customAfter completion of the reaction
  3. customresulting in a substantial amount of precipitate
  4. filtrationThen, the precipitate was suction-filtered
  5. customthe filter cake was recrystallized with acetone

출처 및 근거

ORD 기록
ord-4e1a3b5185124e079c66a717fc1b1ff5
출처 데이터셋
uspto-grants-2015_02
특허 번호
US08946436B2

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