HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diethyl 4,4-difluoroheptanedioate → Ethyl 5,5-difluoro-2-oxocyclohexane-1-carboxylate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diethyl 4,4-difluoroheptanedioate | HCID 10264195 | — |
| Reactant | Potassium tert-butoxide | HCID 23665647 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | Ethyl 5,5-difluoro-2-oxocyclohexane-1-carboxylate | HCID 53362434 | — |
Reaction Steps
To a solution of diethyl 4,4-difluoroheptanedioate (4.3 g) in toluene (50 mL) was added potassium 2-methylpropan-2-olate (2.87 g) and the reaction stirred overnight at room temperature. The reaction was quenched with 1N aqueous HCl (100 mL) and extracted with diethyl ether (150 mL). The ether layer was washed with brine (50 mL), dried over magnesium sulfate, filtered, and concentrated. Silica gel chromatography (Reveleris 40 g) eluting with a gradient of 1% to 5% ethyl acetate/hexanes gave the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09045420B2 |
| Source dataset | uspto-grants-2015_06 |
| ORD ID | ord-8d23b60f806643acb55e9ffb2a7d4360 |
| Source note | uspto-grants-2015_06 |