関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1,4-Dibromobenzene | HCID 7804 | — |
| 反応物 | 3-methylAzetidine | HCID 19995942 | — |
| 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 | 1-(4-Bromophenyl)-3-methylazetidine | HCID 81615982 | 84.74% |
反応手順
3-methylazetidine (0.5 g, 4.69 mmol), diacetoxypalladium (10.53 mg, 0.05 mmol), 2,2'-bis(diphenylphosphino)-1,1'-binaphthyl (0.058 g, 0.09 mmol) and cesium carbonate (3.67 g, 11.26 mmol), degassed toluene (15 mL) were heated at 100 °C over the weekend. The RM was filtered and washed with EtOAc the filtrate was then concentrated and the crude product purified by flash silica chromatography, elution gradient 20 to 30% EtOAc in heptane. Purest fractions were collected and combined with EN05604-93. The combined product was then recrystalised from EtOAc to give 1-(4-bromophenyl)-3-methylazetidine (0.899 g, 85 %).
情報源と証拠
| 出典データセット | 750 AstraZeneca ELN dataset |
|---|
| ORD ID | ord-1e9ec853eb3e43adb71af85c977827e9 |
|---|
| 出典メモ | 750 AstraZeneca ELN dataset |
|---|