HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diethyl (ethoxymethylene)malonate → Ethyl 2-(3,5-difluorophenyl)-1,6-dihydro-1-(2-methoxyethyl)-6-oxo-5-pyrimidinecarboxylate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diethyl (ethoxymethylene)malonate | HCID 6871 | — |
| Reactant | Sodium ethoxide | HCID 2723922 | — |
| Reactant | HCID 178495960 | HCID 178495960 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | Ethyl 2-(3,5-difluorophenyl)-1,6-dihydro-1-(2-methoxyethyl)-6-oxo-5-pyrimidinecarboxylate | HCID 67955325 | — |
Reaction Steps
To a stirred solution of 3,5-difluoro-N-(2-methoxyethyl)benzenecarboximidamide hydrochloride (1:1 (i.e. the product from Example 9, Step B) (24.3 mmol) in ethanol (25 mL) was added diethyl ethoxymethylenemalonate (5.25 g, 24.3 mmol) followed by sodium ethoxide (21% soln) (9.1 mL, 24.3 mmol). The reaction mixture was heated and stirred at reflux for 24 h. The reaction mixture was cooled to room temperature concentrated under reduced pressure. The residue was purified by column chromatography eluting with 50% ethyl acetate in hexanes to afford the title product as a white solid (6.1 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09187432B2 |
| Source dataset | uspto-grants-2015_11 |
| ORD ID | ord-d89deebd92c740dc88e3c6509576e898 |
| Source note | uspto-grants-2015_11 |