HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 19423537, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Trichloroacetyl chloride | HCID 6420 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | (2-Aminopyridin-3-yl)(phenyl)methanone | HCID 12711129 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 19423537 | HCID 19423537 | 72.7% |
Reaction Steps
To a solution of 11.0 g (55 mmol) of 2-amino-3-benzoylpyridine and 6.1 g (60 mmol) of triethylamine in 200 mL of tetrahydrofuran was added dropwise 10.0 g (55 mmol) of trichloroacetyl chloride at temperature of 5° to 15° C. After being stirred for 3 hours at ambient temperature, the reaction mixture was poured into water, and then the mixture was extracted with ethyl acetate. The organic layer separated was washed with water and then with brine, dried on anhydrous sodium sulfate and then concentrated in vacuo. The resulting crude crystals were recrystallized from ethanol to give 14.0 g (40 mmol) of the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05556860 |
| Source dataset | uspto-grants-1996_09 |
| ORD ID | ord-4874c90b9eff49d0b491d0986763490c |
| Source note | uspto-grants-1996_09 |