HuagongsheHuagongshe Chemistry Print Report · For research reference only
Phosphorus oxychloride → 4-Chloro-2-(trifluoromethyl)pyrimidine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Phosphorus oxychloride | HCID 24813 | — |
| Reactant | HCID 178516506 | HCID 178516506 | — |
| Product | 4-Chloro-2-(trifluoromethyl)pyrimidine | HCID 15294369 | — |
Reaction Steps
To 2-(trifluoromethyl)pyrimidin-4-ol (2 g, 12 mmol) was added POCl3 (15 mL). It was refluxed overnight. The solvent was removed. 1N NaOH was added to the reaction mixture slowly until pH=10. The mixture was extracted with DCM (3×80 mL). Combined DCM layer dried over Na2SO4 and taken to dryness. The crude product was vacuum distilled. 4-chloro-2(trifluoromethyl)pyrimidine was obtained as a clear oil. (94%). 1H NMR (400 MHz, DCM) δ: 7.60 (d, J=3 Hz, 1H), 8.80 (d, J=3 Hz, 1H),
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08530652B2 |
| Source dataset | uspto-grants-2013_09 |
| ORD ID | ord-f2e15707bd564309ab7cccc581dfe216 |
| Source note | uspto-grants-2013_09 |