HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Phosphorus oxychloride → 2-Chloro-4,5-diphenylpyrimidine
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Phosphorus oxychloride | HCID 24813 | — |
| Edukt | Phosphorus pentachloride | HCID 24819 | — |
| Edukt | 5,6-Diphenyl-1-methyl-2(1H)-pyrimidinone | HCID 3609352 | — |
| Produkt | 2-Chloro-4,5-diphenylpyrimidine | HCID 12674276 | — |
Reaktionsschritte
A solution of 1-methyl-5,6-diphenyl-1H-pyrimidin-2-one (106, 314 mg, 1.20 mmol), phosphorus oxychloride (0.6 ml, 6.4 mmol) and phosphorus pentachloride (55 mg, 0.26 mmol) was heated at 120° C. for 3 hours. The excess amount of phosphorus oxychloride was removed under reduced pressure and cold water was added to the residue. The resulting precipitate was extracted with CH2Cl2. The organic layer was washed with brine, and dried over MgSO4, and concentrated in vacuo. The residue was purified by column chromatography (20% ethyl acetate in hexane) to produce the title compound as a white solid.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07728014B2 |
| Quelldatensatz | uspto-grants-2010_06 |
| ORD ID | ord-c92f9d8542fc4ac49029ecc678997a58 |
| Quellennotiz | uspto-grants-2010_06 |