HuagongsheHuagongshe Chemistry Print Report · For research reference only
Phosphorus oxychloride → HCID 22648011, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Phosphorus oxychloride | HCID 24813 | — |
| Reactant | HCID 178503547 | HCID 178503547 | — |
| Product | HCID 22648011 | HCID 22648011 | — |
Reaction Steps
A solution of 5.9 g of 6-(2,4-difluorophenyl)-5-methyl-2-(methylthio)pyrimidin-4-ol in 25 mL of POCl3 was heated to reflux and stirred at this temperature for 5 h. All but ca. 5 mL of POCl3 was removed by vacuum distillation, and the residue was quenched by pouring into 200 mL of ice-water, neutralizing with Na2CO3 and extracting with 3×100 mL of EtOAc. The combined organics were washed with 100 mL of brine, dried, and concentrated. The residue was purified by flash chromatography on a Biotage 40M column, eluting with 95:5 hexanes-acetone to yield the title compound as a light yellow solid. Mass spectrum (ESI) 287 (M+1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06809199B2 |
| Source dataset | uspto-grants-2004_10 |
| ORD ID | ord-6344ea63a6984fb2ba644e1be184b4cc |
| Source note | uspto-grants-2004_10 |