HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 66654601, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Acetoxyacetyl chloride | HCID 26297 | — |
| Reactant | 2-Amino-5-(trifluoromethyl)pyridine | HCID 735862 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 66654601 | HCID 66654601 | 40.9% |
Reaction Steps
Triethylamine (9.30 g, 91.9 mmol) was added at 0° C. to a stirred solution of 2-amino-5-trifluoromethylpyridine (5.0 g, 30.8 mmol) in DCM, and stirring was continued for 15 min. 2-Chloro-2-oxoethyl acetate (5.03 g, 36.8 mmol) was added at 0° C., and the temperature was raised to room temperature and the mixture was stirred for 4 hrs. The reaction mixture was diluted with DCM and washed with ice-water, aq. NaHCO3 solution and saturated brine solution, dried over anhydrous Na2SO4, and concentrated under reduced pressure to afford the crude compound. This was purified by column chromatography (100-200 silica gel), eluting with 0-20% EtOAc/pet ether to give the title compound (3.30 g) as a pale brown solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09115132B2 |
| Source dataset | uspto-grants-2015_08 |
| ORD ID | ord-a693338e6661429987ccd3bbe9fb3fc6 |
| Source note | uspto-grants-2015_08 |