HuagongsheHuagongshe Chemistry Print Report · For research reference only
Phosphorus oxychloride → HCID 178430308, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Phosphorus oxychloride | HCID 24813 | — |
| Reactant | 2-(4-Chloro-phenyl)-5-methyl-3H-pyrimidin-4-one | HCID 59906611 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 178430308 | HCID 178430308 | 92% |
Reaction Steps
2-(4-Chloro-phenyl)-5-methyl-3H-pyrimidin-4-one (570 mg, 2.58 mmol) was suspended in phosphorus oxychloride (2 ml) and heated to reflux for 2 hours. The mixture was cooled before being stripped to dryness in vacuo. The resulting crude product was solubilised in water (10 ml) and ethyl acetate (10 ml) and the biphasic mixture separated. The aqueous layer was further extracted with ethyl acetate (10 ml) before the combined organics were dried with magnesium sulphate, filtered and stripped to dryness in vacuo to give 6-Chloro-2-(4-chloro-phenyl)-5-methyl-1,6-dihydro-pyrimidine as a white solid (567 mg, 2.38 mmol, 92% yield).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09051300B2 |
| Source dataset | uspto-grants-2015_06 |
| ORD ID | ord-70814a55b4ad43909d17efb6c68b6058 |
| Source note | uspto-grants-2015_06 |