Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Malonic Acid | HCID 867 | — |
| Reactant | Piperidine | HCID 8082 | — |
| Reactant | HCID 19972556 | HCID 19972556 | — |
| Solvent | Pyridine | HCID 1049 | — |
| Product | HCID 19972449 | HCID 19972449 | — |
Reaction Steps
A mixture of 7.92 g of 8-formyl-3-methyl-4-oxo-2-phenyl-4H-1-benzopyran (prepared as described in Uneyama, K. et al., Bull. Chem. Soc. Jap. 58.; 2361, (1985)) 3.75 g of malonic acid and 0.46 ml of piperidine in 15 ml of anhydrous pyridine was stirred at 100° C. for 3 hours. After cooling to 20°-25° C. the reaction mixture was poured into a mixture of 90 g of crushed ice and 33 ml of hydrochloric acid (d=1.18). The resultant precipitate was collected by suction filtration, washed with water and crystallized twice from 95% ethanol to give 5.5 g of the title compound, m.p. 226°-229° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05605896 |
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| Source dataset | uspto-grants-1997_02 |
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| ORD ID | ord-c95f0f58920c4301a2c4e74ceec8141f |
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| Source note | uspto-grants-1997_02 |
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