Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Nitrogen → [4'-(8,12b-Diazabenzo[a]aceanthrylen-8-yl)biphenyl-4-yl]diphenylamine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Nitrogen | HCID 947 | — |
| 반응물 | Tris(1,1-dimethylethyl)phosphine | HCID 83681 | — |
| 반응물 | 4-Bromo-4'-(diphenylamino)biphenyl | HCID 11315550 | — |
| 반응물 | Sodium t-butoxide | HCID 23676156 | — |
| 반응물 | 8H-8,12b-Diazabenzo[a]aceanthrylene | HCID 67110567 | — |
| 촉매 | palladium(II) acetate | HCID 167845 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | 1,4-Dioxane | HCID 31275 | — |
| 생성물 | [4'-(8,12b-Diazabenzo[a]aceanthrylen-8-yl)biphenyl-4-yl]diphenylamine | HCID 67324186 | — |
반응 단계
A degassed solution of 35.6 g (89 mmol) of (4′-bromobiphenyl-4-yl)-diphenylamine and 22.0 g (81 mmol) of 8H-8,12b-diazabenzo[a]aceanthrylene in 1000 ml of dioxane is saturated with N2 for 1 h. Then firstly 1.0 ml (4 mmol) of P(tBu)3, then 0.4 g (2 mmol) of palladium(II) acetate are added to the solution, and 11.7 g (122 mmol) of NaOtBu in the solid state are subsequently added. The reaction mixture is heated under reflux for 18 h. After cooling to room temperature, 1000 ml of water are carefully added. The organic phase is separated off, washed with 4×50 ml of water and dried over MgSO4, and the solvent is removed in vacuo. The pure product is obtained by recrystallisation and final sublimation in a high vacuum.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US09133119B2 |
| 출처 데이터셋 | uspto-grants-2015_09 |
| ORD ID | ord-ecf6fc362d3a484090a4aaeee18f7bf1 |
| 출처 메모 | uspto-grants-2015_09 |