HRID3318
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customThe solvent was removed
- customthe solid was crystallized from MeOH/Et2O
- customdried