反应详情

温度

100 °C

To a solution of 2-{(S)-1-[(3R,4S)-1-benzyl-4-(3,4-difluoro-phenyl)-pyrrolidin-3-yl]ethoxy}-5-chloro-pyridine 917 mg (2.13 mmol) dissolved in toluene (20 mL) were added 0.69 mL (6.39 mmol) of 1-chloroethyl chloroformate and 1.09 mL (6.39 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 (20 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 464 mg (64%) of the title compound as a light yellow oil. ES-MS m/e: 339.1 (M+H+).

1. temperatureAfter cooling down to RT
2. customvolatiles were removed under vacuo
3. dissolutionthe crude was dissolved in MeOH (20 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)