Reaktionsgleichung
[F:1][C:2]1[CH:3]=[C:4]([NH:26][C:27]([C:29]2[O:30][CH:31]=[CH:32][CH:33]=2)=[O:28])[CH:5]=[C:6]2[C:10]=1[N:9](C(C1OC=CC=1)=O)[N:8]=[C:7]2/[CH:18]=[CH:19]/[C:20]1[CH:21]=[N:22][CH:23]=[CH:24][CH:25]=1.N>C(O)C.[Cl-].[Na+].O>[F:1][C:2]1[CH:3]=[C:4]([NH:26][C:27]([C:29]2[O:30][CH:31]=[CH:32][CH:33]=2)=[O:28])[CH:5]=[C:6]2[C:10]=1[NH:9][N:8]=[C:7]2[CH:18]=[CH:19][C:20]1[CH:21]=[N:22][CH:23]=[CH:24][CH:25]=1Komponenten
Edukt 2
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 2
Versuchsvorschrift
208 mg of furan-2-carboxylic acid{7-fluoro-1-(furan-2-carbonyl)-3-[(E)-2-(pyridin-3-yl)-vinyl]-1H-indazol-5-yl}-amide was suspended in 20 mL ethanol, added with 5 mL of concentrated aqueous ammonia and stirred at room temperature overnight. The reaction solution was added with saturated brine, extracted with ethyl acetate, and the organic phase was washed with saturated brine, and dried over magnesium sulfate. The solvent was evaporated, purified by LC-MS and the obtained crystals were suspended in ethyl acetate, neutralized with saturated aqueous sodium hydrogen carbonate, and the organic phase was washed with water and saturated brine, and dried over magnesium sulfate. The solvent was evaporated, to afford 96.2 mg of the title compound as yellow crystals.
Aufarbeitung
- extractionextracted with ethyl acetate
- washthe organic phase was washed with saturated brine
- dry with materialdried over magnesium sulfate
- customThe solvent was evaporated
- custompurified by LC-MS
- washthe organic phase was washed with water and saturated brine
- dry with materialdried over magnesium sulfate
- customThe solvent was evaporated
Quellen und Nachweise
- ORD-Eintrag
- ord-e573073fc06345ba9a52f5d3cadd9a76
- Quelldatensatz
- uspto-grants-2008_09
- Patentnummer
- US07429609B2
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