참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Piperazine | HCID 4837 | — |
| 반응물 | tert-butyl N-(5-bromo-2-chlorophenyl)carbamate | HCID 57840526 | — |
| 시약 | Cesium carbonate | HCID 10796 | — |
| 촉매 | Binap, (A+-)- | HCID 634876 | — |
| 촉매 | Palladium (II) acetate | HCID 4144353 | — |
| 용매 | Toluene | HCID 1140 | — |
| 생성물 | tert-butyl N-[2-chloro-5-(piperazin-1-yl)phenyl]carbamate | HCID 57840409 | 57.11% |
반응 단계
palladium(II) acetate (0.110 g, 0.49 mmol), BINAP (0.244 g, 0.39 mmol) and CS2CO3 (1.594 g, 4.89 mmol) were added to a mixture of [Reactants] and piperazine (2.76 g, 32.10 mmol) in toluene (10 mL), The suspension were heated to 110 °C for 16 hours, LCMS showed product mass [M+1]:312.0 at retention time RT=1.69 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 as a yellow solid. LCMS confirmed the target compound.
출처 및 근거
| 출처 데이터셋 | 750 AstraZeneca ELN dataset |
|---|
| ORD ID | ord-839e83634a9943b98e2511e3c8112ffb |
|---|
| 출처 메모 | 750 AstraZeneca ELN dataset |
|---|