Reaktion #1503845
ord-e9b3114c4f9b48da8a8bc8f9380b0853
Reaktionsgleichung
Reagenzien
Keine
Reaktionsbedingungen
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1SonstigeSolvent was removed
- 2Sonstigethe remaining white solid was recrystallized from methanol/Et2O
Vorschrift
The compound from step 109c (338 mg, 1.45 mmol) was slurried in ether (15 mL), and ether saturated with HCl gas was added. Solvent was removed and the remaining white solid was recrystallized from methanol/Et2O to give 317 mg of short white needles, 81% yield. m.p. =181-182° C. MS (CI) m/e 233 (M+H)+. 1H NMR (20, 300 MHz) δ: 8.13 (d, J=2.9 Hz, 1H), 7.79 (d, J=2.9 Hz, 1H), 4.99-4.91 (m, 1H), 4.44 (d, J=4.4 Hz, 2H), 4.21-4.03 (m, 2H), 2.74-2.65 (m, 2H). Anal. calc. for C9H11Cl3N2O: C, 40.10; H, 4.11; N, 10.39; Found: C, 39.89; H, 4.08; N, 10.25.