反应详情

温度

0 °C

7a-(3-methyl-5-isoxazolyl)-hexahydro-1H-pyrrolizine (from step 1e, 189 mg, 0.98 mmol) was immersed in Et2O (7 mL) and cooled to 0° C. A solution of Et2O saturated with HCl (g) was added to the reaction vessel dropwise with stirring. The solvent was carefully removed and the remaining white solid triturated with Et2O (2×) followed by recrystallization out of MeOH/Et2O (126.5 mg, 56%). mp 169°-171° C. MS (CI/NH3) m/e: 193 (M+H)+. 1H NMR (D2O, 300 MHz) δ2.20-2.41 (m, 9H), 2.60-2.68 (m, 2H), 3.31-3.39 (m, 2H), 3.71-3.79 (m, 2H), 6.59 (s, 1H). Anal. Calcd for C11H17ClN2O: C, 57.76; H, 7.49; N, 12.25. Found: C, 57.84; H, 7.34; N, 12.13.

1. customThe solvent was carefully removed
2. customthe remaining white solid triturated with Et2O (2×)
3. customfollowed by recrystallization out of MeOH/Et2O (126.5 mg, 56%)