化工社化工社 化学情報印刷レポート · 研究参考用
Hydrochloric Acid → Ethyl 6-chloro-4-[2-fluoro-4-(1,1,2,2,3,3,4,4,4-nonafluorobutyl)anilino]nicotinate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Ethyl 4,6-dichloropyridine-3-carboxylate | HCID 600045 | — |
| 反応物 | 2-Fluoro-4-(nonafluorobutyl)aniline | HCID 23630910 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | Ethyl 6-chloro-4-[2-fluoro-4-(1,1,2,2,3,3,4,4,4-nonafluorobutyl)anilino]nicotinate | HCID 23631003 | 30% |
反応手順
2-Fluoro-4-(1,1,2,2,3,3,4,4,4-nonafluorobutyl) aniline and ethyl 4,6-dichloronicotinate were reacted in a mixture of EtOH and conc. HCl for 36 h as for example 33, step A. The resultant solid was purified by flash chromatography on silica gel (Hexane—10% EtOAc/Hexane gradient elution) to give ethyl 6-chloro-4-[2-fluoro-4-(1,1,2,2,3,3,4,4,4-nonafluorobutyl)anilino]nicotinate (30%). 1H NMR [400 MHz, CDCl3] δ 10.11 (br s, 1H), 8.86 (s, 1H), 7.57 (t, J=8.0 Hz, 1H), 7.46 (d, J=9.7 Hz, 2H), 6.98 (d, J=0.7 Hz, 1H), 4.44 (q, J=7.1 Hz, 2H), 1.44 (t, J=7.1 Hz, 3H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07273877B2 |
| 出典データセット | uspto-grants-2007_09 |
| ORD ID | ord-9ac626bc22f244ae95eb51bffae07469 |
| 出典メモ | uspto-grants-2007_09 |