関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | Tetrahydro-4H-pyran-4-ol | HCID 74956 | — |
| 反応物 | 5-Bromo-2-chloropyridine | HCID 2734414 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 5-Bromo-2-(tetrahydro-2H-pyran-4-yloxy)pyridine | HCID 21914391 | 79.2% |
反応手順
tetrahydro-2H-pyran-4-ol (850 mg, 8.32 mmol) was dissolved in DMF (10 mL), cooled to 0° C., NaH (500 mg, 10.4 mmol) was added and stirred for 45 minutes at room temperature, then 5-bromo-2-chloropyridine (2 g, 10.4 mmol) was added and the mixture was stirred overnight at 60° C. The mixture was poured into water, extracted by EA, the organic layer was washed by brine, dried over Na2SO4, concentrated and purified by flash chromatography, gave 1.7 g white solid. MS: (m/z): 258 (M−H)+, 260 (M+H)+
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US09434726B2 |
|---|
| 出典データセット | uspto-grants-2016_09 |
|---|
| ORD ID | ord-7694a110ba134784a421258096b9983e |
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| 出典メモ | uspto-grants-2016_09 |
|---|
