HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrogen Bromide → HCID 5330212, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrogen Bromide | HCID 260 | — |
| Reactant | HCID 5330211 | HCID 5330211 | — |
| Solvent | Propionic Acid | HCID 1032 | — |
| Product | HCID 5330212 | HCID 5330212 | 46% |
Reaction Steps
A mixture of 8-ethyl-2-(4-methoxyphenylamino)-8H-pyrido[2,3-d]pyrimidin-7-one (133 mg, 0.45 mmol) and 1 mL of 48% aqueous HBr in 10 mL of propionic acid was heated at reflux for 3 hours. After cooling to room temperature, the reaction mixture was partitioned between ethyl acetate and saturated sodium bicarbonate. The aqueous layer was further extracted with ethyl acetate and the organic layers were combined and washed with brine, dried over magnesium sulfate, filtered, and concentrated in vacuo. The resultant solid was purified by dissolving in ethyl acetate and passing the solution through silica gel to provide 58 mg (46%) of 8-ethyl-2-(4 hydroxyphenylamino)-8H-pyrido[2,3-d]pyrimidin-7-one, mp 222-224° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06498163B1 |
| Source dataset | uspto-grants-2002_12 |
| ORD ID | ord-eeee8c9d21d34fb592aac50afa0338c1 |
| Source note | uspto-grants-2002_12 |