Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Potassium Carbonate → 3,5-Dimethyl-6-phenanthridinamine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | 2-Bromo-4,6-dimethylaniline | HCID 170579 | — |
| 반응물 | 2-(2-Cyanophenyl)-4,4,5,5-tetramethyl-1,3,2-dioxaborolane | HCID 3570229 | — |
| 반응물 | Toluene methanol | HCID 21867641 | — |
| 촉매 | HCID 178418397 | HCID 178418397 | — |
| 생성물 | 3,5-Dimethyl-6-phenanthridinamine | HCID 57453549 | 82% |
반응 단계
Added together 2-cyanophenylboronic acid pinacol ester (13.7 g, 60 mmol), 2-bromo-4,6-dimethylaniline (10.0 g, 50 mmol), tetrakis(triphenylphosphine)palladium(0) (2.3 g, 2.0 mmol) and potassium carbonate (18.6 g, 138.21 mol) to a 125 mL of a 95/5 mixture of toluene/methanol. The solvents were degassed and the reaction mixture heated to reflux for 48 hours. After cooling, the reaction mixture was vacuum filtered and the organics evaporated and crude product was purified using silica gel column chromatography treated with triethylamine and 1:9 ethyl acetate and methylene chloride mixture as the eluants. The pure product was collected and concentrated to give 3,5-dimethyl-6-phenanthridinamine (9.1 g, 82% Yield).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08889864B2 |
| 출처 데이터셋 | uspto-grants-2014_11 |
| ORD ID | ord-851f03fadd004f01bc2eab46cd2b8c8b |
| 출처 메모 | uspto-grants-2014_11 |