Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Diethyl Ether | HCID 3283 | — |
| Reactant | Ethyl Acetoacetate | HCID 8868 | — |
| Reactant | Methyl 3-aminocrotonate | HCID 643918 | — |
| Reactant | 3-Ethynylbenzaldehyde | HCID 2771644 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 19813408 | HCID 19813408 | 68.8% |
Reaction Steps
In 20 ml of ethyl alcohol was dissolved 1.95 g (15 mmol) of 3-ethynylbenzaldehyde. Thereto were added 1.73 g (15 mmol) of methyl 3-aminocrotonate and 1.95 g (15 mmol) of ethyl acetoacetate. The mixture was stirred with heating for 16 hours at 80° C. After completing the reaction, the reaction solution was concentrated. The obtained precipitate was washed with ether and then recrystallized from the mixture solution of n-pentane and diethylether (n-pentane: diethylether =3 : 1 (by volume, hereinafter the same)) to give 3.5 g of the desired compound as yellow needle crystals (yield: 70%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05158963 |
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| Source dataset | uspto-grants-1992_10 |
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| ORD ID | ord-06c94c4fe8a24e6bb687b4e6d64a558c |
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| Source note | uspto-grants-1992_10 |
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