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Triethylamine → 1-[4-Hydroxy-4-(3-(trifluoromethyl)phenyl)-1-piperidinyl]-2-(6-benzimidazolyl)-1-ethanone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 4-[3-(Trifluoromethyl)phenyl]-4-piperidinol | HCID 75255 | — |
| 反応物 | Benzotriazol-1-yloxy-tris(dimethylamino)phosphonium hexafluorophosphate | HCID 151348 | — |
| 反応物 | 2-(1H-Benzo[d]imidazol-6-yl)acetic acid | HCID 3046611 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 1-[4-Hydroxy-4-(3-(trifluoromethyl)phenyl)-1-piperidinyl]-2-(6-benzimidazolyl)-1-ethanone | HCID 178520193 | — |
反応手順
A mixture of 1.46 g (0.0083 mol) of 1H-benzimidazol-6-ylacetic acid from preparation 3, 2.0 g (0.0081 mol) of 4-hydroxy-4-(3-(trifluoromethyl)phenyl)piperidine, 3.6 g of BOP and 3.4 ml of triethylamine in 40 ml of dimethylformamide is stirred at ambient temperature overnight. A mixture of ethyl acetate and of water is added, the two phases are separated, the organic phase is dried over sodium sulfate and the solvent is evaporated. The crude product is purified by chromatography on a column of silica gel, elution being carried out with an ethyl acetate/methanol=9/1 mixture, and the title compound is thus obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07186720B2 |
| 出典データセット | uspto-grants-2007_03 |
| ORD ID | ord-26c678bbe47845178a2d85dbbf176f86 |
| 出典メモ | uspto-grants-2007_03 |