化工社化工社 化学情報印刷レポート · 研究参考用
Water → Methyl 6-chloro-4-cyano-2-(4-fluoro-3-methylphenylamino)nicotinate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 4-Fluoro-m-toluidine | HCID 67981 | — |
| 反応物 | Methyl 2,6-dichloro-4-cyanonicotinate | HCID 58317683 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | Methyl 6-chloro-4-cyano-2-(4-fluoro-3-methylphenylamino)nicotinate | HCID 58317541 | — |
反応手順
A solution of methyl 2,6-dichloro-4-cyanonicotinate (500 mg, 2.164 mmol), 4-fluoro-3-methylaniline (325 mg, 2.60 mmol) and Et3N (0.452 mL, 3.25 mmol) in ACN (5 mL) was stirred at 50° C. for 24 h. Water and EtOAc were added to the mixture and the aqueous phase was extracted with EtOAc. The organic phases were combined, washed with H2O and brine, dried over MgSO4, and evaporated. The residue was purified by chromatography on SiO2 to give the title compound, which contains some starting material and was used without further purification (390 mg). [M+H] calc'd for C15H11ClFN3O2, 320. found, 320.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09181255B2 |
| 出典データセット | uspto-grants-2015_11 |
| ORD ID | ord-331a83e14590484ab21628e242de4e27 |
| 出典メモ | uspto-grants-2015_11 |