HuagongsheHuagongshe Chemistry Print Report · For research reference only
Toluene → HCID 22660237, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Toluene | HCID 1140 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Phosphorus oxychloride | HCID 24813 | — |
| Reactant | HCID 86589859 | HCID 86589859 | — |
| Solvent | Sodium chloride; water | HCID 57417360 | — |
| Product | HCID 22660237 | HCID 22660237 | 49.9% |
Reaction Steps
A mixture of 3-[4-chloro-2-fluoro-5-(2-pyrimidinyloxy)phenyl]-6-trifluoromethyl-2,4(1H,3H)-pyrimidinedione(2.01 g, 0.005 mol), phosphorus oxychloride (3.83 g, 0.025 mol), triethylamine (2.02 g, 0.02 mol and toluene (7 ml) was heated under reflux for 2 hours. The reaction mixture was poured into brine, and extracted with ethyl acetate. The organic phase was separated, dried over anhydrous sodium sulfate, and concentrated. The residue was purified by column chromatography on silica gel(40% ethyl acetate/hexane) to give compound III-2 (1.05 g, yield 49.9%) as a white solid, m.p.132-134.5° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06806367B2 |
| Source dataset | uspto-grants-2004_10 |
| ORD ID | ord-d8df4718b1da4d3a9f69b953c7d7bfa7 |
| Source note | uspto-grants-2004_10 |