HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Potassium Carbonate → 3,5-Dimethyl-6-phenanthridinamine
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Potassium Carbonate | HCID 11430 | — |
| Edukt | 2-Bromo-4,6-dimethylaniline | HCID 170579 | — |
| Edukt | 2-(2-Cyanophenyl)-4,4,5,5-tetramethyl-1,3,2-dioxaborolane | HCID 3570229 | — |
| Edukt | Toluene methanol | HCID 21867641 | — |
| Katalysator | HCID 178418397 | HCID 178418397 | — |
| Produkt | 3,5-Dimethyl-6-phenanthridinamine | HCID 57453549 | 82% |
Reaktionsschritte
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).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08889864B2 |
| Quelldatensatz | uspto-grants-2014_11 |
| ORD ID | ord-851f03fadd004f01bc2eab46cd2b8c8b |
| Quellennotiz | uspto-grants-2014_11 |