Reaktionsgleichung
[CH:1]1([C:4]([NH:6][C:7]2[N:31]=[C:10]3[CH:11]=[CH:12][C:13]([O:15][C:16]4[CH:17]=[C:18]([NH:23]C(=O)OC(C)(C)C)[CH:19]=[CH:20][C:21]=4[CH3:22])=[CH:14][N:9]3[N:8]=2)=[O:5])[CH2:3][CH2:2]1.FC(F)(F)C(O)=O>>[NH2:23][C:18]1[CH:19]=[CH:20][C:21]([CH3:22])=[C:16]([CH:17]=1)[O:15][C:13]1[CH:12]=[CH:11][C:10]2[N:9]([N:8]=[C:7]([NH:6][C:4]([CH:1]3[CH2:3][CH2:2]3)=[O:5])[N:31]=2)[CH:14]=1Komponenten
3
Reaktionsbedingungen
- Temperatur
- 0 °C
Versuchsvorschrift
A mixture of tert-butyl [3-({2-[(cyclopropylcarbonyl)amino][1,2,4]triazolo[1,5-a]pyridin-6-yl}oxy)-4-methylphenyl]carbamate (1.50 g, 3.54 mmol) and trifluoroacetic acid (5 mL) was stirred at 0° C. for 30 min. The solvent was evaporated under reduced pressure, and the residue was dissolved in water, neutralized with saturated aqueous sodium hydrogen carbonate solution, and extracted with ethyl acetate. The organic layer was washed with water and saturated brine, dried over anhydrous magnesium sulfate and filtrated. The filtrate was concentrated under reduced pressure, and the residue was collected by filtration and washed with ethyl acetate-hexane to give the title compound (1.04 g, 91%) as a white solid.
Aufarbeitung
- customThe solvent was evaporated under reduced pressure
- dissolutionthe residue was dissolved in water
- extractionextracted with ethyl acetate
- washThe organic layer was washed with water and saturated brine
- dry with materialdried over anhydrous magnesium sulfate
- filtrationfiltrated
- concentrationThe filtrate was concentrated under reduced pressure
- filtrationthe residue was collected by filtration
- washwashed with ethyl acetate-hexane
Quellen und Nachweise
- ORD-Eintrag
- ord-49c190ef76cf4217944ec2bfa2ebc491
- Quelldatensatz
- uspto-grants-2012_11
- Patentnummer
- US08304557B2
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