HuagongsheHuagongshe Chemistry Print Report · For research reference only
Bromotrimethylsilane → HCID 22630518, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Bromotrimethylsilane | HCID 76113 | — |
| Reactant | HCID 22630503 | HCID 22630503 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 22630518 | HCID 22630518 | 84.2% |
Reaction Steps
To a solution of 11.54 g of 1-(diethylphosphono)-4-(nonafluorobutyl)butane in 50 mL of dichloromethane was added 10.7 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 1 hr, and then concentrated to give a white solid. Dissolution in methanol and concentration were repeated two more times, and recrystallization of the crude product from acetonitrile gave 8.39 g of 1-phosphono-4-(nonafluorobutyl)butane (CF3(CF2)3(CH2)4PO3H2) as colorless needles, m.p. 123-124° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06824882B2 |
| Source dataset | uspto-grants-2004_11 |
| ORD ID | ord-448aad817a8e4b7d8b45243c16820de4 |
| Source note | uspto-grants-2004_11 |