Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | Ethyl cyanoacetate | HCID 7764 | — |
| Reactant | Piperidine | HCID 8082 | — |
| Reactant | Veratraldehyde | HCID 8419 | — |
| Solvent | Benzene | HCID 241 | — |
| Product | HCID 68647810 | HCID 68647810 | — |
Reaction Steps
Add 3,4-dimethoxy benzaldehyde 26 g (0.16 mol), ethyl cyanoacetate 18 g (0.16 mol), piperidine 0.8 ml, acetic acid 2.4 g, and benzene 60 ml into 250 ml eggplant-shaped flask, increase temperature to 120-130° C. for intensive reflux, separate water with water separator, react for 12 h. Vacuum evaporate to remove benzene, pour ice water into the reaction solution to precipitate yellow solid, filter and dry to obtain pale yellow crystal VIII-b-2 41 g, with yield almost reaching theoretical value and m.p. 154-156° C. (reference value 156° C.).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07820692B2 |
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| Source dataset | uspto-grants-2010_10 |
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| ORD ID | ord-f47fbf1b13034c2591afff6032fe9456 |
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| Source note | uspto-grants-2010_10 |
|---|