참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Piperazine | HCID 4837 | — |
| 반응물 | 4-Bromo-2-nitrotoluene | HCID 123546 | — |
| 시약 | Cesium carbonate | HCID 10796 | — |
| 촉매 | Binap, (A+-)- | HCID 634876 | — |
| 촉매 | Palladium (II) acetate | HCID 4144353 | — |
| 용매 | Toluene | HCID 1140 | — |
| 생성물 | 1-(4-Methyl-3-nitrophenyl)piperazine | HCID 4738804 | 39.25% |
반응 단계
palladium(II) acetate (0.065 g, 0.29 mmol), BINAP (0.144 g, 0.23 mmol) and CS2CO3 (0.943 g, 2.89 mmol) were added to a mixture of 4-bromo-1-methyl-2-nitrobenzene (0.5 g, 2.31 mmol) and piperazine (1.623 g, 18.84 mmol) . The suspension were heated to 110 °C for 24 hours, LCMS showed product mass [M+1]: 222.1 at retension time RT=1.21 min (polar short purity method). Workup reaction by additional of water (10mL), extracted with EtOAc (3x20 mL), washed with brine, dried with Na2SO4, evaporated off solvent to give a residue, which was purified by isco chromatographer, eluting with 0-10% MeOH in DCM to give 1-(4-methyl-3-nitrophenyl)piperazine (0.201 g, 39.3 %) as a yellow solid.
출처 및 근거
| 출처 데이터셋 | 750 AstraZeneca ELN dataset |
|---|
| ORD ID | ord-7a7d88bb15974f808c2ac9e73fb46a04 |
|---|
| 출처 메모 | 750 AstraZeneca ELN dataset |
|---|