HuagongsheHuagongshe Chemistry Print Report · For research reference only
Perfluorobutyl iodide → 1-(2-Methyl-1,3-dioxolan-2-yl)-alpha-(1,1,2,2,3,3,4,4,4-nonafluorobutyl)cyclopropanemethanol
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Perfluorobutyl iodide | HCID 67917 | — |
| Reactant | 1-(2-Methyl-1,3-dioxolan-2-YL)cyclopropane-1-carbaldehyde | HCID 14375557 | — |
| Reactant | HCID 178419607 | HCID 178419607 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Product | 1-(2-Methyl-1,3-dioxolan-2-yl)-alpha-(1,1,2,2,3,3,4,4,4-nonafluorobutyl)cyclopropanemethanol | HCID 22614418 | — |
Reaction Steps
1.2 g of 97 and 3.92 ml of perfluorobutyl iodide in 40 ml of diethyl ether are introduced under argon and methyllithium/lithium bromide complex (1.5 M in diethyl ether) is added in drops at −78° C. After 30 minutes, it is quenched with sodium chloride solution and diluted with ethyl acetate. Extraction with ethyl acetate, washing of the combined organic phases with sodium chloride solution, drying on sodium sulfate, removal of the solvent and chromatography on silica gel with ethyl acetate/hexane yields 2.1 g of 1-(2-methyl-1,3-dioxolan-2-yl)-α-(1,1,2,2,3,3,4,4,4-nonafluorobutyl)cyclopropanemethanol 98 as a colorless oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06376480B1 |
| Source dataset | uspto-grants-2002_04 |
| ORD ID | ord-42402f6f06fa421ea9fddd945be55418 |
| Source note | uspto-grants-2002_04 |