HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Carbonate → HCID 68209594, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 1-(2,5-Difluorophenyl)ethan-1-one | HCID 74794 | — |
| Reactant | HCID 178418936 | HCID 178418936 | — |
| Solvent | N-methyl-2-pyrrolidone | HCID 13387 | — |
| Product | HCID 68209594 | HCID 68209594 | 35% |
Reaction Conditions
| Temperature | 140 °C |
|---|
Reaction Steps
To a solution of 2′,5′-difluoroacetophenone (10.0 g, 64 mmol) in 1-methyl-2-pyrrolidinone (10 mL) was added potassium carbonate (8.84 g, 64 mmol) and 1H-1,2,3-triazole (6.64 g, 96 mmol). This mixture was heated to 140° C. for 3 hr, under an atmosphere of nitrogen. After this time, the reaction was cooled and then partitioned between ethyl acetate (300 mL) and aqueous ammonium chloride solution (1M, 100 mL). The organic phase was washed with water (3×200 mL) and then dried over magnesium sulphate, filtered and concentrated under reduced pressure. The residue was purified by chromatography on silica gel eluting with ethyl acetate in heptane (10:90 by volume) to produce the title compound as a brown oil (4.6 g, 35%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08916593B2 |
| Source dataset | uspto-grants-2014_12 |
| ORD ID | ord-a94988ef766644ef9b662f2c3dd35fd7 |
| Source note | uspto-grants-2014_12 |