Reaktionsgleichung
[C:1]([O:5][C:6]([NH:8][C:9]1[CH:28]=[N:27][CH:26]=[CH:25][C:10]=1[C:11]([NH:13][C:14]1[CH:19]=[C:18]([C:20]([F:23])([F:22])[F:21])[CH:17]=[CH:16][C:15]=1O)=[O:12])=[O:7])([CH3:4])([CH3:3])[CH3:2].O1CCCC1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.N(C(OCC)=O)=NC(OCC)=O>C1(C)C=CC=CC=1>[C:1]([O:5][C:6]([NH:8][C:9]1[CH:28]=[N:27][CH:26]=[CH:25][C:10]=1[C:11]1[O:12][C:15]2[CH:16]=[CH:17][C:18]([C:20]([F:21])([F:23])[F:22])=[CH:19][C:14]=2[N:13]=1)=[O:7])([CH3:3])([CH3:2])[CH3:4]Komponenten
6
Edukt 4
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Versuchsvorschrift
To a mixture of 1.78 g of 3-tert-butoxycarbonylamino-N-[2-hydroxy-5-(trifluoromethyl)phenyl]isonicotinamide, 20 ml of tetrahydrofuran and 1.29 g of triphenylphosphine, 2.15 g of 40% toluene solution of diethyl azodicarboxylate was added dropwise at room temperature. The reaction mixture was stirred at room temperature for one hour and then stirred while heating at 50° C. for 30 minutes. The reaction mixture was cooled to room temperature, and then concentrated under reduced pressure. The residue was subjected to silica gel column chromatography to give 0.69 g of 2-(3-tert-butoxycarbonylamino pyridin-4-yl)-5-(trifluoromethyl)benzoxazole (hereinafter, referred to as “active compound 36”).
Aufarbeitung
- additionwas added dropwise at room temperature
- stirringstirred
- temperaturewhile heating at 50° C. for 30 minutes
- temperatureThe reaction mixture was cooled to room temperature
- concentrationconcentrated under reduced pressure
Quellen und Nachweise
- ORD-Eintrag
- ord-72ea188dabb541058694b5d925e24a9a
- Quelldatensatz
- uspto-grants-2012_12
- Patentnummer
- US08324387B2
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