関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2-Bromopyridine | HCID 7973 | — |
| 反応物 | (6-Aza-spiro[2.5]oct-1-yl)-(4-cyclobutyl-piperazin-1-yl)-methanone | HCID 59395236 | — |
| 試薬 | Sodium t-butoxide | HCID 23676156 | — |
| 触媒 | Palladium (II) acetate | HCID 4144353 | — |
| 触媒 | 2-Dicyclohexylphosphino-2',4',6'-triisoprophylbiphenyl | HCID 11155794 | — |
| 生成物 | (4-Cyclobutyl-piperazin-1-yl)-(6-pyridin-2-yl-6-aza-spiro[2.5]oct-1-yl)-methanone | HCID 25119543 | 9.39% |
反応手順
Reagents were put in a sealed vial and heated in the microwave oven for 10 minutes at 160°C. According to LC-MS analysis, the conversion is >90%. The crude mixture was transferred to a round-bottomed flask and volatiles were evaporated under vacuum. The residue was purified on preparative HPLC using the long high pH (acetonitrile in water ammonium carbonate buffer, 25 min.) 20 to 40% gradient method on XBridge Prep C18 OBD, 30x150 mm, 5 mm, Waters reverse phase column, giving (4-cyclobutylpiperazin-1-yl)(6-(pyridin-2-yl)-6-azaspiro[2.5]octan-1-yl)methanone (7.20 mg, 9.39 %). However, the compound was not pure enought for submission and there was not enough of it to attempt another purification.
情報源と証拠
| 出典データセット | 750 AstraZeneca ELN dataset |
|---|
| ORD ID | ord-c35b162a34bf408282b33e4af9af7634 |
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| 出典メモ | 750 AstraZeneca ELN dataset |
|---|