HuagongsheHuagongshe Chemistry Print Report · For research reference only
Tetrahydrofuran → 4-(4-Bromo-2-fluorophenylamino)-6-chloro-5-fluoro-nicotinic acid methyl ester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Tetrahydrofuran | HCID 8028 | — |
| Reactant | Trimethylsilyldiazomethane | HCID 167693 | — |
| Reactant | 4-(4-Bromo-2-fluorophenylamino)-6-chloro-5-fluoro-nicotinic acid | HCID 86601526 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | 4-(4-Bromo-2-fluorophenylamino)-6-chloro-5-fluoro-nicotinic acid methyl ester | HCID 86601527 | 92.3% |
Reaction Steps
A hexanes solution of TMSCH2N2 (9.46 mL, 18,9 mmol) was added to 4-(4-bromo-2-fluorophenylamino)-6-chloro-5-fluoro-nicotinic acid (4.59 g, 12.62 mmol) in a solution of 3:1 THF:MeOH (48 mL) at 0° C. The reaction mixture was warmed to room temperature and stirred for 1 hour. After quenching with AcOH, the reaction mixture was diluted with ethyl acetate and water. The layers were separated and the organic layer was washed with water, saturated NaHCO3 solution and brine. The organic layer was dried (MgSO4) and concentrated to give 4.40 g (92%) clean desired product.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07732616B2 |
| Source dataset | uspto-grants-2010_06 |
| ORD ID | ord-a5641726e7bf4352858e1977f38281da |
| Source note | uspto-grants-2010_06 |