反应详情

温度

100 °C

To a solution of 2-{(SR)-1-[(3RS,4SR)-1-benzyl-4-(3,4-dichloro-phenyl)-pyrrolidin-3-yl]-ethoxy}-5-trifluoromethyl-pyridine 0.45 g (0.91 mmol) dissolved in toluene (5 mL) were added 0.30 mL (2.7 mmol) of 1-chloroethyl chloroformate and 0.46 mL of Hunig's base. The reaction mixture was heated at 100° C. for one hour. After cooling down to RT, volatiles were removed under vacuo and the crude was dissolved in MeOH (5 mL). The reaction mixture was heated at 85° C. for 30 minutes and after cooling down to RT, volatiles were removed under vacuo and the residue was directly purified on column chromatography (SiO2, CH2Cl2/MeOH 9:1) yielded 0.32 g (87%) of the title compound as a light yellow oil. ES-MS m/e: 405.9 (M+H+).

1. temperatureAfter cooling down to RT
2. customvolatiles were removed under vacuo
3. dissolutionthe crude was dissolved in MeOH (5 mL)
4. temperatureThe reaction mixture was heated at 85° C. for 30 minutes
5. temperatureafter cooling down to RT
6. customvolatiles were removed under vacuo
7. customthe residue was directly purified on column chromatography (SiO2, CH2Cl2/MeOH 9:1)