HuagongsheHuagongshe Chemistry Print Report · For research reference only
Phosphorus oxychloride → Methyl (4-chloro-6-methyl-2-methylmercapto-5-pyrimidinyl)-acetate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Phosphorus oxychloride | HCID 24813 | — |
| Reactant | HCID 178499514 | HCID 178499514 | — |
| Solvent | N,N-Diethylaniline | HCID 7061 | — |
| Product | Methyl (4-chloro-6-methyl-2-methylmercapto-5-pyrimidinyl)-acetate | HCID 53971641 | 72% |
Reaction Steps
Methyl (4-hydroxy-6-methyl-2-methylmercapto-5-pyrimidinyl)-acetate (4.0 g, 17 mmol) is heated in a mixture of phosphoroxychloride (40 ml) and N,N-diethylaniline (5.5 ml) for 2 hours at 100° C. The excess phosphoroxychloride was removed by evaporation under vacuum and the residue poured into ice-water. Extraction with ethyl acetate, drying and filtration over silicagel gives methyl (4-chloro-6-methyl-2-methylmercapto-5-pyrimidinyl)-acetate as a crystalline solid (3.1 g, 72%), having a m.p. of 88° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05635508 |
| Source dataset | uspto-grants-1997_06 |
| ORD ID | ord-65d223cb18d64e4b918d9e9253e15c7b |
| Source note | uspto-grants-1997_06 |