関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | N-Ethylaniline | HCID 7670 | — |
| 反応物 | 5-Bromo-2-iodo-4-methoxypyrimidine | HCID 84819520 | — |
| 試薬 | Sodium 2-methylbutan-2-olate | HCID 2733478 | — |
| 触媒 | Palladium (II) acetate | HCID 4144353 | — |
| 触媒 | Bis(adamantan-1-yl)(butyl)phosphane | HCID 11371790 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 5-bromo-N-ethyl-4-methoxy-N-phenylpyrimidin-2-amine | HCID 106998693 | 53.74% |
反応手順
5-bromo-2-iodo-4-methoxypyrimidine (0.086 g, 0.27 mmol), diacetoxypalladium (2.78 mg, 0.01 mmol), di((3S,5S,7S)-adamantan-1-yl)(butyl)phosphine (8.88 mg, 0.02 mmol) and sodium 2-methylbutan-2-olate (0.033 g, 0.30 mmol) were added to a micro vial. Then N-ethylaniline (0.031 mL, 0.25 mmol) in toluene (1.5 mL) was added to the reaction mixture. The vial was sealed and evacuated and flushed with nitrogen and then stirred at 60°C o/n. LC/MS showed product formation. The reaction mixture was cooled to rt and then filtered over celite. The crude product was diluted with 25 ml of DCM and then washed with sat. NaHCO3 followed by brine. The organic phase was dried over a phase separator and then concentrated to dryness. **No LC/MS data due to database failure over three months and was only saved locally on LC/MS computer and pdf-files seems to be deleted on machine. Not used in further reactions.**
情報源と証拠
| 出典データセット | 750 AstraZeneca ELN dataset |
|---|
| ORD ID | ord-8bbed4d3f8cb496989e49be7e55b89ca |
|---|
| 出典メモ | 750 AstraZeneca ELN dataset |
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