Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Benzaldehyde | HCID 240 | — |
| Reactant | Diethyl methylmalonate | HCID 11857 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 56923598 | HCID 56923598 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 68565974 | HCID 68565974 | — |
Reaction Steps
Under cooling (0° C.), diethyl methylmalonate ([609-08-5], 1.175 g, 7 mmol) was added to a suspension of NaH (60% in mineral oil, 325 mg, 8 mmol) in diethyl ether (30 ml). After 3 h at r.t, the solvent was evaporated and the residue was dissolved in DMF (20 ml). To this solution, triphenylvinylphosphonium bromide ([5044-52-0], 3.00 g, 8 mmol) and benzaldehyde ([100-52-7], 860 mg, 8 mmol) were added. The reaction mixture was stirred at 100° C. overnight, and was then taken up in ethyl acetate, washed (H2O), and dried (Na2SO4). The solvent was evaporated, and 2-methyl-2-(3-phenyl-allyl)-malonic acid diethyl ester was isolated from the residue by column chromatography (silica gel, ethyl acetate/heptane). MS: m/e=291.0 [M+H+].
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07572801B2 |
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| Source dataset | uspto-grants-2009_08 |
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| ORD ID | ord-851eba3b5c484275b878ee1db49f750f |
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| Source note | uspto-grants-2009_08 |
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