HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 21876400, compound → HCID 21875606, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 21876400 | HCID 21876400 | — |
| Solvent | Hydrochloric Acid | HCID 313 | — |
| Product | HCID 21875606 | HCID 21875606 | 71.2% |
Reaction Steps
A mixture of diethyl 2-(6-{[4-(2-hydroxyethyl)phenyl]amino}-2-methyl-5-nitro-4-pyrimidinyl)propanedioate (step 2, 2.0 g, 6.48 mmol) in 2N aqueous HCl (15 ml) was heated at reflux temperature for 5 h. After cooling, the reaction was quenched with saturated NaHCO3 aqueous solution (100 ml), and the whole was extracted with ethyl acetate (100 ml×3). The organic layer was washed with brine (50 ml), dried (MgSO4), and concentrated. Purification by flash column chromatography eluting with hexane/ethyl acetate (gradient elution from 1:1 to 0:100) to afford 1.33 g (71%) of the title compound as a yellow solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07141580B2 |
| Source dataset | uspto-grants-2006_11 |
| ORD ID | ord-cd5a192187644f7881dc181152ee962e |
| Source note | uspto-grants-2006_11 |