تفاعل #3385

ord-092e97d5277f41ea9797e8d42117af0e

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىThe solvent was removed
  2. 2
    أخرىthe precipitate was triturated (3×) with Et2O
  3. 3
    أخرىto afford a yellow solid (26 mg, quant)

الإجراء التجريبي

7a-(2-Chloro-3-pyridinyl)-hexahydro-1H-pyrrolizine (21 mg, 0.1 mmol) was dissolved in Et2O (6 mL), and Et2O saturated with HCl (g) was added. The solvent was removed, and the precipitate was triturated (3×) with Et2O to afford a yellow solid (26 mg, quant). mp 186°-188° C. MS (CI/NH3) m/e: 223 (M+H)+. 1H NMR D2O, 300 MHz) δ2.03-2.18 (m, 2H), 2.29-2.41 (m, 2H), 2.54-2.64 (m, 2H), 2.75-2.84 (m,2H), 3.41-2.51 (m, 2H), 2.93-4.02 (m, 2H), 7.57 (dd, J=8.1, 4.7 Hz, 1H), 8.01 (dd, J=8.1, 1.7 Hz, 1H), 8.42 (dd, J=4.7, 1.7 Hz, 1H). Anal. Calcd for Cl2H16Cl2N2 : C, 55.61; H, 6.22; N, 10.81. Found: C, 55.21; H, 6.25; N, 10.45

المصدر

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