HuagongsheHuagongshe Chemistry Print Report · For research reference only
Phosphorus oxychloride → 3-benzyl-6-chloro-5-methylpyrimidine-2,4(1H,3H)-dione
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Phosphorus oxychloride | HCID 24813 | — |
| Reactant | 1-Benzyl-5-methyl-pyrimidine-2,4,6-trione | HCID 18936722 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | 3-benzyl-6-chloro-5-methylpyrimidine-2,4(1H,3H)-dione | HCID 18936885 | — |
Reaction Steps
To 16.8 ml of 50% ethanol, 78.7 ml (844 mmol) of phosphorus oxychloride was added dropwise, with stirring under ice cooling conditions. To this solution, 23.22 g (100 mmol) of 3-benzyl-5-methylpyrimidine-2,4,6(1H,3H)-trione was added little by little. This mixture was stirred at 50° C. for 30 minutes and then at 100° C. for 90 minutes. After cooling, the reaction mixture was poured into ice water and stirred for 1 hour. The resulting precipitate was collected by filtration, washed with water and n-hexane and dried to yield 27.50 g (quant, light white crystal) of the desired product.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05840732 |
| Source dataset | uspto-grants-1998_11 |
| ORD ID | ord-fed3e0ea75bf47e29a61d6f7b0c21785 |
| Source note | uspto-grants-1998_11 |