HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethyl Acetate → HCID 57082426, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | Diethyl (cyanomethyl)phosphonate | HCID 75676 | — |
| Reactant | 7-(Methylsulfanyl)-1,2,3,4-tetrahydronaphthalen-1-one | HCID 21917078 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 57082426 | HCID 57082426 | — |
Reaction Steps
Under an inert atmosphere and at 0° C., diethyl cyanomethylphosphonate (7.6 ml, 46.8 mmol) is added dropwise to a suspension of sodium hydride (2.25 g, 46.8 mmol) in 50 ml of tetrahydrofuran. Stirring is carried out at 0° C. for 30 minutes; the compound obtained in Step C (6 g, 31.2 mmol), dissolved in 50 ml of tetrahydrofuran, is then added and the reaction mixture is stirred at ambient temperature for 3 hours. After hydrolysis and extraction with ethyl acetate, the organic phase is washed with water, dried over magnesium sulphate and evaporated. The residue is purified by chromatography on silica gel (eluant: petroleum ether/dichloromethane 50/50) to yield the unsaturated nitrile of the title.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07115752B2 |
| Source dataset | uspto-grants-2006_10 |
| ORD ID | ord-73b463dbed1f44a6af7dc72822656f43 |
| Source note | uspto-grants-2006_10 |