HRID3318

反应详情

EQUATION

反应方程式

HRID 3318 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

7a-(6-Fluoro-5-methyl-3-pyridinyl)-hexahydro-1H-pyrrolizine (115 mg, 0.52 mmol, from step 18d) was dissolved in Et2O, and Et2O saturated with HCl (g) was added. The solvent was removed, and the solid was crystallized from MeOH/Et2O and dried to afford the title compound (white needles, 92 mg, 69%): mp 170-171° C.; 1H NMR (D2 O, 300 MHz) δ2.12-2.47 (m, 9H), 2.56-2.66 (m, 2H), 3.32-3.41 (m, 2H), 3.77-3.86 (m, 2H), 7.94 (m, 1H), 8.14 (m, 1H); MS (CI/NH3) m/z: 221 (M+H)+ ; MS (CI/NH3): m/z 221 (M+H+). Anal. Calcd for C13H17FN2.HCl: C, 60.82; H, 7.07; N, 10.91. Found: C, 60.83; H, 6.80; N, 10.63.

WORKUP

后处理

  1. customThe solvent was removed
  2. customthe solid was crystallized from MeOH/Et2O
  3. customdried