関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 反応物 | 2-Fluoro-6-methylpyridine | HCID 96090 | — |
| 反応物 | 6-Hydroxy-3,4-dihydro-1(2H)-naphthalenone | HCID 4679494 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 6-[(6-Methylpyridin-2-yl)oxy]-1,2,3,4-tetrahydronaphthalen-1-one | HCID 118597588 | 26.3% |
反応手順
A suspension of 6-hydroxy-1-tetralone (3.0 g, 18 mmol), 2-fluoro-6-methylpyridine (2.06 g, 18.5 mmol) and Cs2CO3 (12.1 g, 37.0 mmol) in DMF (150 mL) was stirred at 150° C. in a sealed vessel overnight under N2. The reaction was poured into water (300 mL) and extracted with EtOAc (3×50 mL). Organics were dried (Na2SO4) and concentrated. Purification by silica gel chromatography (PE:EA=5:1) gave 1.2 g (26%) of the title compound as a red oil. [M+H] calc'd for C16H15NO2, 254. found 254.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US09447046B2 |
|---|
| 出典データセット | uspto-grants-2016_09 |
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| ORD ID | ord-c3f01bbcdaaa4bc2b954cfbe82a1dec0 |
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| 出典メモ | uspto-grants-2016_09 |
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