참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Piperazine | HCID 4837 | — |
| 반응물 | 5-Bromo-2,2-difluoro-1,3-benzodioxole | HCID 2736271 | — |
| 시약 | Potassium tert-butoxide | HCID 23665647 | — |
| 촉매 | Tris(1,1-dimethylethyl)phosphine | HCID 83681 | — |
| 촉매 | Bis(tri-tert-butylphosphine)palladium(0) | HCID 2734558 | — |
| 용매 | 1,4-Dioxane | HCID 31275 | — |
| 생성물 | 1-(2,2-Difluoro-2H-1,3-benzodioxol-5-YL)piperazine | HCID 21363750 | 50.68% |
반응 단계
13-May-09 10:32:07 +0100 5-bromo-2,2-difluorobenzo[d][1,3]dioxole (0.500 g, 2.11 mmol), piperazine (0.182 g, 2.11 mmol) and BIS(TRI-T-BUTYLPHOSPHINE)PALLADIUM(0) (0.054 g, 0.11 mmol) and potassium 2-methylpropan-2-olate (0.349 g, 2.95 mmol) were suspended in dioxane (10vol) (10 mL) and heated to 90°C for 1 hour. LC-MS shows no starting material 52% product and 41% dimer. The reaction mixture was combined with EN02263-54 filtered and the crude product was purified by flash silica chromatography, elution gradient 0 to 10% MeOH in DCM. Pure fractions were evaporated to dryness to afford 1-(2,2-difluorobenzo[d][1,3]dioxol-5-yl)piperazine (0.259 g, 50.7 %) as a yellow oil.
출처 및 근거
| 출처 데이터셋 | 750 AstraZeneca ELN dataset |
|---|
| ORD ID | ord-a6f7db18dd5949e09df857ba4df0f8b1 |
|---|
| 출처 메모 | 750 AstraZeneca ELN dataset |
|---|
