Reaktionsgleichung
[N:1]1[CH:6]=[CH:5][CH:4]=[C:3]([NH:7][S:8]([C:11]2[CH:20]=[CH:19][CH:18]=[CH:17][C:12]=2[C:13]([O:15]C)=O)(=[O:10])=[O:9])[CH:2]=1.[F:21][C:22]1[CH:23]=[C:24]([CH:27]=[CH:28][CH:29]=1)[CH2:25][NH2:26]>>[F:21][C:22]1[CH:23]=[C:24]([CH:27]=[CH:28][CH:29]=1)[CH2:25][NH:26][C:13](=[O:15])[C:12]1[CH:17]=[CH:18][CH:19]=[CH:20][C:11]=1[S:8]([NH:7][C:3]1[CH:2]=[N:1][CH:6]=[CH:5][CH:4]=1)(=[O:9])=[O:10]Komponenten
Versuchsvorschrift
The title compound was prepared according to procedures described above, using methyl 2-[(pyridin-3-ylamino)sulfonyl]benzoate and 3-fluorobenzylamine. The title compound was further purified by dissolving 25 g in EtOH (300 mL) and gently heating using water bath to 80° C. The resulting solids material were then slowly dissolved and more EtOH (50 mL) was added to completely dissolve all the solids. The solution left at room temperature to crystallize for 1 h. The resulting crystals were collected and dried under high vacuum for 16 h to afford the title compound as a crystalline solid (21 g, 84%). 1H NMR (400 MHz, DMSO-D6) δ 9.76 (s, 1H) 9.32 (t, 1H) 8.31 (d, 1H) 8.25 (d, 1H) 7.66-7.78 (m, 2H) 7.50-7.65 (m, 3H) 7.39 (q, 1H) 7.23-7.29 (m, 3H) 7.09 (t, 1H) 4.54 (d, 2H).
Aufarbeitung
- customThe title compound was prepared
- customThe title compound was further purified
- dissolutionby dissolving 25 g in EtOH (300 mL)
- temperaturegently heating
- customto 80° C
- dissolutionThe resulting solids material were then slowly dissolved
- additionmore EtOH (50 mL) was added
- dissolutionto completely dissolve all the solids
- waitThe solution left at room temperature
- customto crystallize for 1 h
- customThe resulting crystals were collected
- customdried under high vacuum for 16 h
Quellen und Nachweise
- ORD-Eintrag
- ord-e51005026b8440159f1ae8ed703df0c1
- Quelldatensatz
- uspto-grants-2011_01
- Patentnummer
- US07868026B2
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