反应详情

To a solution of 14.6 g (35 mmol) of 1-(diethylphosphono)-3,7,11,15-tetramethylhexadecane in 40 mL of dichloromethane was added 15.0 g (98 mmol) of bromotrimethylsilane. After 24 h at room temperature, the solution was concentrated to a pale yellowish liquid, and the intermediate silylphosphonate ester was dissolved in 100 mL of methanol. The resultant solution was stirred at room temperature for 30 min and concentrated to a white solid. Dissolution in methanol and concentration were repeated two times, and recrystallization from ethyl acetate afforded 10.5 g (83%) of 1-phosphono-3,7,11,15-tetramethylhexadecane as white crystals, mp 69-72° C.

1. concentrationthe solution was concentrated to a pale yellowish liquid
2. dissolutionthe intermediate silylphosphonate ester was dissolved in 100 mL of methanol
3. concentrationconcentrated to a white solid
4. dissolutionDissolution in methanol
5. concentrationconcentration
6. customtwo times, and recrystallization from ethyl acetate