Bromotrimethylsilane → HCID 22630495, compound

Participants

Reaction Steps

To a solution of 18.63 g of 1-(diethylphosphono)-6-(nonafluorobutyl)hexane in 100 mL of dichloromethane was added 16.8 g of bromotrimethylsilane. After 18 hr at room temperature, the solution was concentrated to a nearly colorless liquid, and the intermediate silylphosphonate ester was dissolved in 250 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 two recrystallizations of the crude product from a 99:1 mixture of heptane and 2-propanol gave 12.50 g of 1-phosphono-6-(nonafluorobutyl)hexane (CF3(CF2)3(CH2)6PO3H2) as colorless leaves, m.p. 107-108° C.

Provenance & Evidence