HuagongsheHuagongshe Chemistry Print Report · For research reference only
Urea → 5-(2-chlorophenyl)pyrimidine-2,4(1H,3H)-dione
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Urea | HCID 1176 | — |
| Reactant | Sodium Iodide | HCID 5238 | — |
| Reactant | Chlorotrimethylsilane | HCID 6397 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Methyl 2-(2-chlorophenyl)-3-(dimethylamino)acrylate | HCID 67505122 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | 5-(2-chlorophenyl)pyrimidine-2,4(1H,3H)-dione | HCID 22064485 | 66.5% |
Reaction Steps
To a mixture of methyl 2-(2-chlorophenyl)-3-(dimethylamino)acrylate 6b (0.26 g, 1.08 mmol), urea (0.2 g, 3.26 mmol) and NaI (0.49 g, 3.26 mmol) in acetonitrile (5 mL) was added TMSCl (0.41 mL, 3.26 mmol). The resulting mixture was refluxed for 16 hours, cooled to room temperature, and 1.0 M NaOH (8 mL) was added. The resultant solution was stirred for 20 hr, and acetonitrile was removed in vacuo. The aq. solution was washed with ether, cooled in ice bath, and neutralized with 1 N HCl (8 mL). The precipitate was filtered, washed with additional H2O, and dried to give 5-(2-chlorophenyl)pyrimidine-2,4(1H,3H)-dione 6c (0.16 g, 66%) as a white solid. MS (CI) m/z 222.9, 224.9 (MH+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07419983B2 |
| Source dataset | uspto-grants-2008_09 |
| ORD ID | ord-87a35943d460418ea8f022473784260a |
| Source note | uspto-grants-2008_09 |