Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | Trimethyl phosphonoacetate | HCID 80029 | — |
| Reactant | 1-(2-Methyl-1,3-dioxolan-2-YL)cyclopropane-1-carbaldehyde | HCID 14375557 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 69650637 | HCID 69650637 | — |
Reaction Steps
3 g of sodium hydride suspension (60% in paraffin oil) is introduced into 750 ml of THF, cooled under nitrogen to 0° C., and 10.9 g of dimethylphosphonoacetic acid methyl ester is added. Then, 7.5 g of aldehyde 7 is added in drops to 15 ml of THF, and it is stirred at room temperature for 2 hours. It is now quenched carefully with sodium chloride solution, extracted with ethyl acetate, washed with sodium chloride solution, dried on sodium sulfate, and the solvent is removed. The residue is chromatographed on silica gel with ethyl acetate/hexane, whereby 9.5 g of title compound 93 accumulates as a colorless oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US07071344B1 |
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| Source dataset | uspto-grants-2006_07 |
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| ORD ID | ord-471da5d51b6b4cea9d594e1b3d56f24b |
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| Source note | uspto-grants-2006_07 |
|---|