化工社化工社 化学情報印刷レポート · 研究参考用
Diisopropylethylamine → 1-[2-(Methylsulfonyl)-4-(trifluoromethoxy)benzoyl]-4-(1-methyl-1-{[3-(trifluoromethyl)phenyl]sulfonyl}ethyl)piperidine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | Benzotriazol-1-yloxy-tris(dimethylamino)phosphonium hexafluorophosphate | HCID 151348 | — |
| 反応物 | HCID 59447309 | HCID 59447309 | — |
| 反応物 | 4-(1-Methyl-1-{[3-(trifluoromethyl)phenyl]sulfonyl}ethyl)piperidine | HCID 59447409 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Trifluoroacetic acid | HCID 6422 | — |
| 生成物 | 1-[2-(Methylsulfonyl)-4-(trifluoromethoxy)benzoyl]-4-(1-methyl-1-{[3-(trifluoromethyl)phenyl]sulfonyl}ethyl)piperidine | HCID 25255784 | — |
反応手順
To a 10 ml vial was added 4-(1-methyl-1-{[3-(trifluoromethyl)phenyl]sulfonyl}ethyl)piperidine (70.8 mg, 0.211 mmol), 2-(methylsulfonyl)-4-(trifluoromethoxy)benzoic acid (50 mg, 0.176 mmol), Bop reagent (93 mg, 0.211 mmol), diisopropylethyl amine (0.062 ml, 0.352 mmol) and 2 ml dimethylformamide. The resulting solution was stirred at room temperature for 10 minutes. The reaction mixture was diluted with 1 ml dimethyl sulfoxide, 1 ml water and 0.03 ml of trifluoroacetic acid. This mixture was loaded on a reverse phase column and purified with HPLC eluted with water/acetonitrile gradient solvent. Desired fraction was collected and lyophilized to give to give title compound as fluffy white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08304434B2 |
| 出典データセット | uspto-grants-2012_11 |
| ORD ID | ord-66f474659cc04294a5f14145823fbc0c |
| 出典メモ | uspto-grants-2012_11 |