Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
1-Iodo-3-nitrobenzene → Tert-butyl 4-(3-nitrophenyl)piperazine-1-carboxylate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 1-Iodo-3-nitrobenzene | HCID 12574 | — |
| 반응물 | Tri-o-tolylphosphine | HCID 80271 | — |
| 반응물 | tert-Butyl piperazine-1-carboxylate | HCID 143452 | — |
| 반응물 | Sodium t-butoxide | HCID 23676156 | — |
| 촉매 | Bis(dibenzylideneacetone)palladium | HCID 9811564 | — |
| 용매 | Diethyl Ether | HCID 3283 | — |
| 용매 | 1,4-Dioxane | HCID 31275 | — |
| 생성물 | Tert-butyl 4-(3-nitrophenyl)piperazine-1-carboxylate | HCID 22330126 | 54% |
반응 단계
To a solution of 1-iodo-3-nitro-benzene (9 g), piperazine-1-carboxylic acid tert-butyl ester (13.5 g) and sodium tert-butoxide (9.7 g) in dioxane (150 mL) was added tris(dibenzylideneacetone)dipalladium (2 g) and tri-o-tolylphosphine (2.2 g) and the mixture was heated at reflux for 24 hours. The solution was then cooled to room temperature, taken in Et2O and washed with brine. The organic layer was dried over Na2SO4, filtered and concentrated under reduced pressure. The crude residue was recrystallized from diisopropyl ether to give the title compound (6 g) as a yellow solid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US06552022B1 |
| 출처 데이터셋 | uspto-grants-2003_04 |
| ORD ID | ord-3e6f4f4adc4544aa9e6884a8a24e610d |
| 출처 메모 | uspto-grants-2003_04 |