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Diisopropylethylamine → 2-[4-(3-Chloropyridin-2-yl)piperazin-1-yl]-6-trifluoromethyl-1H-benzoimidazole
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | 2-chloro-6-(trifluoromethyl)-1H-benzimidazole | HCID 337905 | — |
| 反応物 | 1-(3-Chloropyridin-2-yl)piperazine hydrochloride | HCID 20455074 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 2-[4-(3-Chloropyridin-2-yl)piperazin-1-yl]-6-trifluoromethyl-1H-benzoimidazole | HCID 11710679 | — |
反応手順
A mixture of the hydrochloride salt from step (b) above (0.564 g, 2.4 mmol), 2-chloro-6-trifluoromethyl-1H-benzoimidazole (0.27 g, 1.22 mmol, Example 1c) and N,N-diisopropylethylamine (0.84 mL, 4.8 mmol, Aldrich) in MeCN (1 mL) was subjected to microwave irradiation at 180° C. with stirring for 20 min. The solvent was removed in vacuo and the residue was purified by silica gel chromatography, eluting with 30% EtOAc/hexane, to give the title compound as a white solid. M.p. 208-210° C. MS (ESI, pos. ion) m/z: 382 (M+1).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07582761B2 |
| 出典データセット | uspto-grants-2009_09 |
| ORD ID | ord-e5544c1df3904204b9b36f20069d17c1 |
| 出典メモ | uspto-grants-2009_09 |