HuagongsheHuagongshe Chemistry Print Report · For research reference only
Bromotrimethylsilane → HCID 22630513, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Bromotrimethylsilane | HCID 76113 | — |
| Reactant | HCID 22630506 | HCID 22630506 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 22630513 | HCID 22630513 | 75.6% |
Reaction Steps
To a solution of 7.03 g of 1-(diethylphosphono)-8-(nonafluorobutyl)octane in 30 mL of dichloromethane was added 6.12 g of bromotrimethylsilane. After 18 hr at room temperature, the solution was concentrated to a pale yellow liquid, and the intermediate silylphosphonate ester was dissolved in 150 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 acetonitrile gave 4.68 g of 1-phosphono-8-(nonafluorobutyl)octane (CF3(CF2)3(CH2)8PO3H2) as white crystals, m.p. 87-89° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06824882B2 |
| Source dataset | uspto-grants-2004_11 |
| ORD ID | ord-89b84894020b4497a20051ff572a3832 |
| Source note | uspto-grants-2004_11 |