Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sulfuric Acid | HCID 1118 | — |
| Reactant | Phosphorus oxide (P4O10) | HCID 14812 | — |
| Reactant | HCID 67099636 | HCID 67099636 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 67099917 | HCID 67099917 | — |
Reaction Steps
Diethyl 2-(4-phenyl-tetrahydro-2H-pyran-4-carbonyl)malonate (418 mg, 1200 μmol) was dissolved in a minimal amount of EtOAc and then cooled to 0° C. A slurry of P2O5 (681 mg) and H2SO4 (640 μL, 11998 μmol) (also at 0° C.) was added to the mixture via spatula, and the reaction mixture was stirred for 3 hours. The reaction mixture was then poured into a beaker of ice, diluted with 100 mL of EtOAc, added to a separatory funnel, partitioned with water, washed with water (2×50 mL), separated, dried over Na2SO4, and concentrated in vacuo to give the title compound which was used without further purification. MS m/e=303 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07928139B2 |
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| Source dataset | uspto-grants-2011_04 |
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| ORD ID | ord-6a3ed0f29faf4a1fa58c0dd777365d68 |
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| Source note | uspto-grants-2011_04 |
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