化工社化工社 化学情報印刷レポート · 研究参考用
1,3-Cyclohexanediol → (3-hydroxycyclohexyl) 2-(4-fluoroanilino)-4-oxo-5-(1H-pyrrolo[2,3-b]pyridin-3-ylmethylidene)furan-3-carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1,3-Cyclohexanediol | HCID 10433 | — |
| 反応物 | ethyl 2-(4-fluoroanilino)-4-oxo-5-(1H-pyrrolo[2,3-b]pyridin-3-ylmethylidene)furan-3-carboxylate | HCID 178469558 | — |
| 触媒 | Zinc | HCID 23994 | — |
| 溶媒 | Dimethylacetamide | HCID 31374 | — |
| 生成物 | (3-hydroxycyclohexyl) 2-(4-fluoroanilino)-4-oxo-5-(1H-pyrrolo[2,3-b]pyridin-3-ylmethylidene)furan-3-carboxylate | HCID 178524383 | 13% |
反応手順
A solution of the compound (0.10 g, 0.25 mmol) of Example 21, 1,3-cyclohexanediol (0.44 g, 3.8 mmol) and zinc cluster catalyst (Zn4(OCOCF3)6O) (0.018 g, 0.019 mmol) in N,N-dimethylacetamide (1.0 mL) was stirred at 130° C. for 1.5 days. Cooled to ambient temperature, the precipitate was removed by filtration. The filtrate was purified by preparative HPLC to afford the titled compound as solid (0.010 g, y. 13%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08742113B2 |
| 出典データセット | uspto-grants-2014_06 |
| ORD ID | ord-aa96d85647734d7882ecbe0903cc6797 |
| 出典メモ | uspto-grants-2014_06 |