HuagongsheHuagongshe Chemistry Print Report · For research reference only
Pyridine → HCID 86625499, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | 2,2,2-Trichloroethyl chloroformate | HCID 87063 | — |
| Reactant | 5-Amino-2-(trifluoromethyl)pyridine | HCID 2737744 | — |
| Solvent | Dimethylacetamide | HCID 31374 | — |
| Product | HCID 86625499 | HCID 86625499 | — |
Reaction Steps
To a solution of 6-(trifluoromethyl)pyridine-3-amine (1.00 g, 6.15 mmol) and pyridine (1.50 ml, 18.5 mmol) in N,N-dimethylacetamide (20 ml) was added 2,2,2-trichloroethyl chloroformate (1.17 ml, 8.51 mmol) with ice-cooling, and the mixture was stirred for 1 hour with ice-cooling. The reaction mixture was poured into ice-water and the mixture was extracted with ethyl acetate. The extract was washed with water and dried over anhydrous magnesium sulfate and the solvent was distilled off under reduced pressure. The residue was recrystallized from a mixed solvent of hexane and ethyl acetate and the desired product (1.83 g, 88.0%) as a solid was collected by filtration.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07851473B2 |
| Source dataset | uspto-grants-2010_12 |
| ORD ID | ord-de11db280c3b4e44919bbf2497eb54fb |
| Source note | uspto-grants-2010_12 |