HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethyl 2-(4-oxocyclohexyl)acetate → HCID 11095257, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethyl 2-(4-oxocyclohexyl)acetate | HCID 12666966 | — |
| Reactant | Potassium tert-butoxide | HCID 23665647 | — |
| Catalyst | Methyltriphenyliphosphonium bromide | HCID 74505 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 11095257 | HCID 11095257 | 73.7% |
Reaction Steps
To a cooled (0° C.) suspension of methyl triphenylphosphonium bromide (8.58 g, 23.5 mmol) in THF (60 mL) was added KOtBu (3.17 g, 28.3 mmol) in portions under N2. The reaction was slowly warmed to rt and stirred for 1 h. The resulting mixture was cooled to 0° C. and added a solution of ethyl 2-(4-oxocyclohexyl)acetate (2.9 g, 15.7 mmol) in THF (15 mL). The resulting mixture was stirred at RT for 2 h and at 50° C. overnight. After cooling to RT, the reaction was quenched by addition of saturated NH4Cl, extracted with EtOAc, washed with brine, dried over Na2SO4. Purification by flash column chromatography (eluent: 20% EtOAc in hexanes) gave the product as colorless oil (2.11 g, 73.7%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08912169B2 |
| Source dataset | uspto-grants-2014_12 |
| ORD ID | ord-43d45a5307d144d5bc4beaeb1cc4fb8a |
| Source note | uspto-grants-2014_12 |