Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Aniline | HCID 6115 | — |
| Reactant | HCID 10409330 | HCID 10409330 | — |
| Product | HCID 10412291 | HCID 10412291 | — |
Reaction Steps
The mixture of (±)-7-chloro-1,3-bis-(4-methoxy-phenyl)-4-methyl-3,4-dihydro-1H-pyrimido[4,5-d]pyrimidin-2-one (0.30 g; 0.72 mmol) (from Example 4a supra) and aniline (0.20 mL; 2.16 mmol) (Aldrich) was heated at 100° C. for 40 minutes. The mixture was then cooled to room temperature and triturated with hexanes. The resulting solid was dissolved in dichloromethane, washed with water and brine, dried over sodium sulfate and concentrated. The residue was purified by flash chromatography (Biotage, 12S, dichloromethane followed by 30:70 to 50:50 ethyl acetate-hexanes gradient) to give (±)-1,3-bis-(4-methoxy-phenyl)-4-methyl-7-phenylamino-3,4-dihydro-1H-pyrimido[4,5-d]pyrimidin-2-one. (Yield 0.303 g; 90.1%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US07112676B2 |
|---|
| Source dataset | uspto-grants-2006_09 |
|---|
| ORD ID | ord-77c66e929b4f4e84a41ddece92292cb8 |
|---|
| Source note | uspto-grants-2006_09 |
|---|