Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Diethyl Oxalate | HCID 7268 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 10037388 | HCID 10037388 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 70295804 | HCID 70295804 | — |
Reaction Steps
3-(2-Fluoro-biphenyl-4-yl)-butan2-one (Japanese Patent Unexamined Publication No. 54-144347) (116 mg) was dissolved in toluene (2 ml), followed by adding thereto sodium hydride (29 mg, 60% oily), and the mixture was stirred at room temperature for 1 hour. Then, diethyl oxalate (105 mg) was added and the resulting mixture was stirred at 40° C. for 3 hours. Water was added to the reaction mixture, followed by extraction with ethyl acetate, and the extract solution was washed with water and dried. The solvent was distilled off under reduced pressure and the residue was purified by a silica gel column chromatography to obtain the desired compound (163 mg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US06100260 |
|---|
| Source dataset | uspto-grants-2000_08 |
|---|
| ORD ID | ord-e0f9e46adc364cb4a0808bde7c344e35 |
|---|
| Source note | uspto-grants-2000_08 |
|---|