関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | tert-Butyl carbamate | HCID 77922 | — |
| 反応物 | 2-Chloro-3-fluoro-5-methylpyridine | HCID 13541365 | — |
| 試薬 | Cesium carbonate | HCID 10796 | — |
| 触媒 | 1,1'-(9,9-Dimethyl-9H-xanthene-4,5-diyl)bis(1,1-diphenylphosphine) | HCID 636044 | — |
| 触媒 | Palladium (II) acetate | HCID 4144353 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | tert-butyl N-(3-fluoro-5-methyl-2-pyridinyl)carbamate | HCID 90064798 | 25.74% |
反応手順
diacetoxypalladium (15.42 mg, 0.07 mmol) and(9,9-dimethyl-9H-xanthene-4,5-diyl)bis(diphenylphosphine) (39.8 mg, 0.07 mmol) were added to a degassed mixture of 2-chloro-3-fluoro-5-methylpyridine (100 mg, 0.69 mmol), tert-butyl carbamate (121 mg, 1.03 mmol) and cesium carbonate (336 mg, 1.03 mmol) in dioxane (10 mL) at 21°C. The resulting mixture was stirred at 100 °C for 16 hours.Filtered through celite and adsorbed onto silica. The crude product was purified by flash silica chromatography, elution gradient 0 to 50% DCM in heptane. Pure fractions were evaporated to dryness to afford sm by HNMR Abandoned. ..
情報源と証拠
| 出典データセット | 750 AstraZeneca ELN dataset |
|---|
| ORD ID | ord-e2551fd8964c4f0a80ff232c25d61d8a |
|---|
| 出典メモ | 750 AstraZeneca ELN dataset |
|---|