HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → 2-Chloro-3-nitro-5-(trifluoromethyl)pyridine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Phosphorus oxychloride | HCID 24813 | — |
| Reactant | HCID 178526653 | HCID 178526653 | — |
| Catalyst | Benzyltrimethylammonium chloride | HCID 5963 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | 2-Chloro-3-nitro-5-(trifluoromethyl)pyridine | HCID 4736950 | 92% |
Reaction Steps
In a 25 ml flask, 3-nitro-5-trifluoromethyl-pyridin-2-ol (300 mg, 1.44 mmol) was dissolved in acetonitrile (4.5 ml), and then phosphorus oxychloride (0.4 ml, 4.33 mmol) and benzyltrimethyl ammonium chloride (164 mg, 0.721 mmol) were added thereto. The mixture was stirred for 3 hours at 800. After completion of the reaction, water was added thereto and the mixture was extracted with ethyl acetate. The combined organic layer was dried over anhydrous sodium sulfate (Na2SO4), filtered and evaporated under reduced pressure to obtain white solid (300 mg, 92%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08394792B2 |
| Source dataset | uspto-grants-2013_03 |
| ORD ID | ord-c94d78fb4d51414eb5351a8269bc40af |
| Source note | uspto-grants-2013_03 |