HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Carbonate → 1-(2-Fluoro-3-methoxy-6-nitrophenyl)propan-2-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 1-(2,3-Difluoro-6-nitrophenyl)propan-2-one | HCID 14268876 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | 1-(2-Fluoro-3-methoxy-6-nitrophenyl)propan-2-one | HCID 22030743 | 73.6% |
Reaction Steps
A mixture of 1-(2,3-difluoro-6-nitrophenyl)-propan-2-one (183 g) and potassium carbonate (100 g) in methanol (1 L) was heated at reflux for 3 h. The reaction mixture was then cooled and concentrated in vacuo to remove most of the methanol. The residue was diluted with ethyl acetate (1 L), filtered and washed with water. The separated aqueous layer was neutralized with 2N HCl and extracted with ethyl acetate (2×500 mL). The combined organic layer was washed with brine, dried (Na2SO4) and concentrated in vacuo to give a brown solid. The solid was triturated with diethyl ether and filtered to provide 1-(2-fluoro-3-methoxy-6-nitrophenyl)-propan-2-one (121 g, 71%) as a yellow solid. LC/MS; (M+H)+=228.2.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06869952B2 |
| Source dataset | uspto-grants-2005_03 |
| ORD ID | ord-5b1368bfe72e488fb70c5e9bcd0e24e6 |
| Source note | uspto-grants-2005_03 |