تفاعل #3384
ord-5d856ea1f5d4426aaad2bca65084aa0a
معادلة التفاعل
الكواشف
لا شيء
ظروف التفاعل
الظروف التفصيلية
See reaction.notes.procedure_details.
المعالجة
- 1أخرىThe solvent was removed
- 2أخرىthe precipitate was recrystallized from MeOH/Et2O
الإجراء التجريبي
7a-(2-fluoro-3-pyridinyl)-hexahydro-1H-pyrrolizine (from step 6a, 59 mg, 0.3 mmol) was dissolved in Et2O (8 mL), and Et2O saturated with HCl (g) was added. The solvent was removed, and the precipitate was recrystallized from MeOH/Et2O to afford a white solid (54 mg, 77%). mp 185°-186° C. MS (CI/NH3) m/e: 207 (M+H)+. 1H NMR D2O, 300 MHz) a 2.06-2.21 (m, 2H), 2.27-2.41 (m, 4H), 2.65-2.77 (m, 2H), 3.32-3.40 (m, 2H), 3.85-3.95 (m, 2H), 7.47 (ddd, J=7.7, 4.8, 1.8 Hz, 1H), 8.14 (ddd, J=10.7, 7.7, 1.8 Hz, 1H), 8.27 (ddd, J=4.8, 1.8, 1.1 Hz, 1H). Anal. Calcd for C12H16ClFN2 : C, 59.38; H, 6.64; N, 11.54. Found: C, 59.14; H, 6.53; N, 11.34.