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Potassium Carbonate → HCID 53699167、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Iodobenzene | HCID 11575 | — |
| 反応物 | 4,7-Dimethoxy-1,10-phenanthroline | HCID 10462298 | — |
| 反応物 | Ethyl 2-oxopiperidine-4-carboxylate | HCID 18699051 | — |
| 触媒 | Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI) | HCID 24350 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | HCID 53699167 | HCID 53699167 | — |
反応手順
Ethyl 2-oxopiperidine-4-carboxylate (0.50 g, 2.9 mmol), iodobenzene (0.77 g, 3.8 mmol, 1.3 equiv), copper(I) iodide (56 mg, 0.29 mmol, 0.1 equiv), 4,7-bis(methoxy)-1,10-phenanthroline (70 mg, 0109 mmol, 0.1 equiv) and potassium carbonate (0.40 g, 3.8 mmol, 1 equiv) were combined in dimethylsulfoxide (10 mL) and placed into a preheated oil bath at 100° C. for 120 hours. The mixture was cooled to ambient temperature, diluted with ethyl acetate (50 mL) and washed with water (2×25 mL) and once with brine (25 mL). The organic extract was dried with sodium sulfate, filtered and concentrated in vacuo, providing the titled compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08895580B2 |
| 出典データセット | uspto-grants-2014_11 |
| ORD ID | ord-65f19b2c707d4e4291724a8b8c599f18 |
| 出典メモ | uspto-grants-2014_11 |