تفاعل #3384

ord-5d856ea1f5d4426aaad2bca65084aa0a

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىThe solvent was removed
  2. 2
    أخرىthe 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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05733912uspto-grants-1998_03