Diisopropylethylamine → N-(3-(1H-pyrazol-3-yl)phenyl)-8-methoxy-2-oxo-2H-chromene-3-carboxamide

HRID 240170

반응식

HRID 240170 반응식
CCN(C(C)C)C(C)C.[CH3:10][O:11][C:12]1[CH:13]=[CH:14][CH:15]=[C:16]2[C:21]=1[O:20][C:19](=[O:22])[C:18]([C:23]([OH:25])=O)=[CH:17]2.CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.[N:50]1[NH:51][C:52]([C:55]2[CH:56]=[C:57]([NH2:61])[CH:58]=[CH:59][CH:60]=2)=[CH:53][CH:54]=1>CN(C=O)C>[N:50]1[NH:51][C:52]([C:55]2[CH:56]=[C:57]([NH:61][C:23]([C:18]3[C:19](=[O:22])[O:20][C:21]4[C:16]([CH:17]=3)=[CH:15][CH:14]=[CH:13][C:12]=4[O:11][CH3:10])=[O:25])[CH:58]=[CH:59][CH:60]=2)=[CH:53][CH:54]=1

참가 물질

6

반응물 4

HCID 81531DiisopropylethylamineHCID 2345628-Methoxy-2-oxo-2H-chromene-3-carboxylic acidHCID 27353983-(1H-Pyrazol-3-yl)anilineHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)

생성물 1

HCID 32205793N-(3-(1H-pyrazol-3-yl)phenyl)-8-methoxy-2-oxo-2H-chromene-3-carboxamide수율 7%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

DIEA (0.011 mL, 0.062 mmol) was added to 8-methoxy-3-carboxy-coumarin (0.012 g, 0.057 mmol) and HATU (0.024 g, 0.062 mmol) in 0.5 mL of DMF with constant stirring at room temperature until a clear solution resulted. Subsequently, 3-(2H-pyrazol-3-yl)-phenylamine (0.009 g, 0.057 mmol) was added and allowed to react overnight when a solid precipitated out of solution. The resulting precipitate was filtered, dried under suction, and finally dried overnight in vacuo to give 0.0014 g of product in 7% yield: LCMS (ESI) m/z 362 (MH+).

후처리

  1. customresulted
  2. customto react overnight when a solid
  3. customprecipitated out of solution
  4. filtrationThe resulting precipitate was filtered
  5. customdried under suction, and finally dried overnight in vacuo

출처 및 근거

ORD 기록
ord-3cb9254f29714e82a57181cb4ce34ec7
출처 데이터셋
uspto-grants-2014_02
특허 번호
US08642788B2

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