HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethyl 4-oxocyclohexanecarboxylate → HCID 18340695, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethyl 4-oxocyclohexanecarboxylate | HCID 317638 | — |
| Reactant | Lithium Chloride | HCID 433294 | — |
| Reactant | tert-Butyl diethylphosphonoacetate | HCID 2773685 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 18340695 | HCID 18340695 | 62.1% |
Reaction Steps
To a suspension of anhydrous lithium chloride (1.9 g, 45 mmol) in MeCN (100 ml) was added tert-butyl 2-(diethoxyphosphoryl)acetate (7.6 g, 30 mmol) at room temperature. The mixture was stirred for 30 min. TEA (6.4 ml, 45 mmol) was added and the mixture was stirred for another 30 min. Ethyl 4-oxocyclohexanecarboxylate (5.1 g, 30 mmol) was added and the mixture was stirred overnight. The precipitate was filtered off and the filtrate was concentrated to afford brown oil, which was purified by silica gel column (PE:EtOAc=10:1) to afford product (5 g, 62%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08759548B2 |
| Source dataset | uspto-grants-2014_06 |
| ORD ID | ord-128e909123a74c0092265e731240ebda |
| Source note | uspto-grants-2014_06 |