HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diethyl phenylmalonate → HCID 178422335, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diethyl phenylmalonate | HCID 66514 | — |
| Reactant | HCID 178418690 | HCID 178418690 | — |
| Solvent | Tributylamine | HCID 7622 | — |
| Product | HCID 178422335 | HCID 178422335 | — |
Reaction Steps
A solution of 4.5 g 5-amino-3-methylpyrazole and 12.2 ml diethyl phenylmalonate in N,N-dibutylbutan-1-amine is stirred at 185° C. over night. After cooling to room temperature the reaction mixture forms two layers. The top layer is removed and the lower layer is diluted with dichloromethane and methanol. The resulting solution is concentrated and extracted with a mixture of diethyl ether and 10% w/w NaOH solution. The organic layer is discarded and aqueous layer acidified with concentrated HCl. The precipitated product is collected by filtration.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08614218B2 |
| Source dataset | uspto-grants-2013_12 |
| ORD ID | ord-f8046eefcd6e49239cc1ec42b4ee26e5 |
| Source note | uspto-grants-2013_12 |