HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethyl 3-oxo-3-(pyridin-3-yl)propanoate → HCID 178426705, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethyl 3-oxo-3-(pyridin-3-yl)propanoate | HCID 222197 | — |
| Reactant | HCID 178426708 | HCID 178426708 | — |
| Solvent | Ethanol | HCID 702 | — |
| Solvent | N-methyl-2-pyrrolidone | HCID 13387 | — |
| Product | HCID 178426705 | HCID 178426705 | — |
Reaction Conditions
| Temperature | 150 °C |
|---|
Reaction Steps
40 g (2-methyl-5-nitrophenyl)guanidine in 160 mL N-methyl pyrrolidone is dissolved. The mixture is heated to 150° C. and ethyl β-oxo-3-pyridine propionate is added portionwise, to 50 g total in a time period of 5 hours, distillating about 15 g of by-products under a nitrogen flow. At the end of the reaction, the mixture is cooled and diluted with ethanol. The precipitate is filtrated, yielding, upon drying, 46.4 g of product with HPLC purity of 99% (A %), identified through LC-MS and 1H-NMR.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08168787B2 |
| Source dataset | uspto-grants-2012_05 |
| ORD ID | ord-543f6e76df6543d6a0ebf8c8e01162ae |
| Source note | uspto-grants-2012_05 |