反应详情

2,4-Dicyanopyridine (601 mg) and ytterbium trifluoromethanesulfonate (289 mg) were added to a solution of (2R)-1,1-bis(4-fluorophenyl)-3-(methoxymethoxy)-1,2-propanediamine (1.50 g) in toluene (30 mL), and the mixture was refluxed under stirring for 2 days. The reaction mixture was concentrated in vacuo, and then the residue was dissolved in tetrahydrofuran (20 mL). 6N Hydrochloric acid (10 mL) was added to the solution, and then the mixture was stirred at room temperature for 24 hours. The reaction mixture was concentrated in vacuo, and then the residue was purified by silica gel column chromatography (C-300; hexane: ethyl acetate=2:1) to give the objective compound (385 mg).

1. temperaturethe mixture was refluxed
2. concentrationThe reaction mixture was concentrated in vacuo
3. dissolutionthe residue was dissolved in tetrahydrofuran (20 mL)
4. addition6N Hydrochloric acid (10 mL) was added to the solution
5. stirringthe mixture was stirred at room temperature for 24 hours
6. concentrationThe reaction mixture was concentrated in vacuo
7. customthe residue was purified by silica gel column chromatography (C-300; hexane: ethyl acetate=2:1)