Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Tetrahydrofuran | HCID 8028 | — |
| Reactant | 1,1,1,3,3,3-Hexafluoro-2-propanol | HCID 13529 | — |
| Reactant | HCID 11804856 | HCID 11804856 | — |
| Reactant | Butyllithium | HCID 178418339 | — |
| Solvent | Hexane | HCID 8058 | — |
| Product | HCID 11515081 | HCID 11515081 | 82.2% |
Reaction Steps
Under nitrogen atmosphere and at 5° C., 129 ml of 1.6M n-butyllithium in hexane was added to a mixture of 16.8 g of 1,1,1,3,3,3-hexafluoro-2-propanol and 120 g of tetrahydrofuran, which was stirred for one hour at 5° C. Next, 14.2 g of 2-oxopropyl methacrylate was added at 5° C. The mixture was stirred for 10 hours, after which dilute hydrochloric acid was added to stop the reaction and neutralize the reaction mixture. Through conventional aqueous work-up and purification by silica gel column chromatography, 25.3 g of the target compound was obtained (yield 82%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US07202318B2 |
|---|
| Source dataset | uspto-grants-2007_04 |
|---|
| ORD ID | ord-2aa5cbab80c548f0966fa19f04514e3e |
|---|
| Source note | uspto-grants-2007_04 |
|---|