HuagongsheHuagongshe Chemistry Print Report · For research reference only
Phosphorus oxychloride → HCID 86662548, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Phosphorus oxychloride | HCID 24813 | — |
| Reactant | HCID 66776516 | HCID 66776516 | — |
| Product | HCID 86662548 | HCID 86662548 | 58.8% |
Reaction Steps
The solution of 2-(2,2,2-trifluoro-ethylsulfanyl)-3H-pyrimidin-4-one (25 g, crude) in POCl3 (250 mL) was stirred and refluxed for 5 hours. After most POCl3 was removed, the residue was dropped into ice and the pH was adjusted to 8-9, extracted with ethyl acetate, dried over MgSO4 and the crude material was purified by column chromatography on silica gel to give 4-chloro-2-(2,2,2-trifluoro-ethylsulfanyl)-pyrimidine (14.6 g, 58.8%) as an oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08765774B2 |
| Source dataset | uspto-grants-2014_07 |
| ORD ID | ord-1a0fc4997c604114b7a073011a67d223 |
| Source note | uspto-grants-2014_07 |