HRID3314

反应详情

EQUATION

反应方程式

HRID 3314 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

7a-(5-bromo-3-pyridinyl)-hexahydro-1H-pyrrolizine (107 mg, 0.52 mmol, from step 16c) was dissolved in methylene chloride, 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 as an off-white powder (118 mg). mp 192°-194° C. 1H NMR D2O, 300 MHz) δ2.13-2.51 (m, 6H), 2.57-2.66 (m, 2H), 3.36-3.44 (m, 2H), 3.81-3.89(m, 2H), 8.22 (s, 1H), 8.65 (s, 1H), 8.72 (s, 1H); MS (CI/NH3) m/z: 267/269 (M+H)+. Anal. Calcd for C12 H15BrN2.HCl: C, 47.47; H, 5.31; N, 9.23. Found: C, 47.40; H, 5.22; N, 8.98.

WORKUP

后处理

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