関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 反応物 | 4-Desoxypyridoxine hydrochloride | HCID 67417 | — |
| 反応物 | 4-Iodobenzonitrile | HCID 76467 | — |
| 反応物 | Dimethylglyoxime | HCID 135459645 | — |
| 触媒 | HCID 178419072 | HCID 178419072 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | HCID 68644271 | HCID 68644271 | 7% |
反応手順
A mixture of 4-deoxypyridoxine hydrochloride (0.44 g, 2.8 mmol), copper (I) oxide (0.50 g, 3.5 mmol), dimethylglyoxime (0.15 g, 1.3 mmol), 4-iodobenzonitrile (1.08 g, 4.7 mmol), cesium carbonate (5.00 g, 15.3 mmol), and crushed molecular sieves 3° A (0.6 g) in anhydrous DMF (4 mL) were heated at 110° C. for 12 hours. The reaction mixture was evaporated to dryness, and the crude product purified by column chromatography on silica gel using a gradient of dichloromethane:methyl alcohol (1:0 to 9:1) as eluant to give 4-(5-hydroxymethyl-2,4-dimethyl-pyridin-3-yloxy)-benzonitrile (89) (50 mg, 7% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07812037B2 |
|---|
| 出典データセット | uspto-grants-2010_10 |
|---|
| ORD ID | ord-5f1d208941b94b31821320586bde4381 |
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| 出典メモ | uspto-grants-2010_10 |
|---|