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2,6-Dibromopyridine → 2-{3-[3,5-Bis(trifluoromethyl)phenyl]-3-(trifluoromethyl)pyrrolidin-1-yl}-6-bromopyridine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2,6-Dibromopyridine | HCID 12274 | — |
| 反応物 | Dimethylacetamide | HCID 31374 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | 3-[3,5-Bis(trifluoromethyl)phenyl]-3-(trifluoromethyl)pyrrolidine | HCID 53262186 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 2-{3-[3,5-Bis(trifluoromethyl)phenyl]-3-(trifluoromethyl)pyrrolidin-1-yl}-6-bromopyridine | HCID 87158573 | 92.3% |
反応手順
A mixture of 3-[3,5-bis(trifluoromethyl)phenyl]-3-(trifluoromethyl)pyrrolidine (3.0 g), 2,6-dibromopyridine (2.22 g), N,N-diisopropylethylamine (2.2 g) and dimethylacetamide (15 ml) was reacted at 160° C. in a sealed tube for 1 hour. Upon the completion of the reaction, the mixture was added with ethyl acetate, washed with water and then saturated brine, dried over anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure. The residue was purified by silica gel chromatography to obtain 2-{3-[3,5-bis(trifluoromethyl)phenyl]-3-(trifluoromethyl)pyrrolidin-1-yl}-6-bromopyridine (4.0 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09375000B2 |
| 出典データセット | uspto-grants-2016_06 |
| ORD ID | ord-2b8d32244fdf469d902e787cde430c9e |
| 出典メモ | uspto-grants-2016_06 |