関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methyl 3-bromobenzoate | HCID 12070 | — |
| 反応物 | 4-(N-Boc-amino)piperidine | HCID 723833 | — |
| 試薬 | Cesium carbonate | HCID 10796 | — |
| 触媒 | Binap, (A+-)- | HCID 634876 | — |
| 触媒 | Palladium (II) acetate | HCID 4144353 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | Methyl 3-{4-[(tert-butoxycarbonyl)amino]piperidin-1-yl}benzoate | HCID 68580036 | 13.76% |
反応手順
All chemicals were mixed in a 50 mL round bottom flask. The solids were degassed and placed under nitrogen. Toluene was added and the mixture was stirred at 100°C for 24 h. Cooled and filtered. The filtrate was concentrated under vacuum. Crude product was mainly starting material but some product had been formed. The product was purified by silica gel chromatography using 1-4% methanol/DCM. Product was slightly more polar than starting material bromide. There was obtained 230 mg of the desired product as a solid. HNMR and LC MS ok.
情報源と証拠
| 出典データセット | 750 AstraZeneca ELN dataset |
|---|
| ORD ID | ord-2de77de369ef42f8b910f9e83130f454 |
|---|
| 出典メモ | 750 AstraZeneca ELN dataset |
|---|
