Trifluoroacetic acid → 1-(5-Chloropyridin-2-yl)piperazine
Reaktionsgleichung
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([N:8]2[CH2:13][CH2:12][N:11](C(OC(C)(C)C)=O)[CH2:10][CH2:9]2)=[N:6][CH:7]=1.FC(F)(F)C(O)=O>>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([N:8]2[CH2:9][CH2:10][NH:11][CH2:12][CH2:13]2)=[N:6][CH:7]=1Komponenten
3
Versuchsvorschrift
Tert-butyl 4-(5-chloropyridin-2-yl)piperazine-1-carboxylate (170 mg, 0.571 mmol) was dissolved in MC (3 ml), followed by addition of trifluoroacetic acid (3 ml), and then the resulting mixture was stirred at room temperature for 2 hours. The resulting reaction liquid was concentrated under reduced pressure, followed by addition of a saturated aqueous NaHCO3 solution (15 ml), and extracted with MC (15 ml×3). The organic layer was dried over anhydrous sodium sulfate, followed by filtration, concentration, and vacuum drying, to obtain 112 mg of white solid (99%).
Aufarbeitung
- customThe resulting reaction liquid
- concentrationwas concentrated under reduced pressure
- additionfollowed by addition of a saturated aqueous NaHCO3 solution (15 ml)
- extractionextracted with MC (15 ml×3)
- dry with materialThe organic layer was dried over anhydrous sodium sulfate
- filtrationfollowed by filtration, concentration, and vacuum
- customdrying
Quellen und Nachweise
- ORD-Eintrag
- ord-f594820042674e4eb2dfcda6c04a5ace
- Quelldatensatz
- uspto-grants-2015_08
- Patentnummer
- US09096571B2
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