With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.12150-46-8,1,1-Bis(diphenylphosphino)ferrocene,as a common compound, the synthetic route is as follows.
1.1 Preparation of N,N’-Di-(o-tolyl)-1,4-phenylenediamine To a 5 L round-bottomed 3-neck flask, equipped with reflux condenser, nitrogen inlet and exhaust, mechanical stirrer (equipped with PTFE stirrer rod, guide and stirrer blade) and a powder addition funnel, was added the 1,4-phenylenediamine (77.85 g, 0.720 mol, 1.0 eq.) and 2-bromotoluene (270.87 g, 1.584 mol, 2.2 eq.) and toluene (1500 mL). The resulting mixture was stirred for 10 mins, then degassed by sparging with nitrogen gas for 1 hour. The palladium(II) acetate (3.60 g, 0.1 eq.) and 1,1′-diphenylphosphinoferrocene (dppf) (8.88 g, 0.1 eq.) were then added and the mixture stirred under nitrogen for 15 mins. Sodium tert-butoxide (207.36 g, 2.16 mol, 3.0 eq.) was then charged as a solid. The mixture was heated to reflux and maintained at this temperature for 16 hours. GCMS after this time indicated complete reaction. The mixture was allowed to cool to room temperature and poured into a mixture of ice-water (1000 mL) and diethyl ether (500 mL). The phases were separated and the organic phase passed through celite (200 g). The filtrates were concentrated to dryness in vacuo and the crude product triturated from methanol. The product was recovered by filtration and the cake washed with methanol (2*250 mL). The solid product was then dried for 24 hours at 40¡ã C. in vacuo. The product was afforded as a pale white solid, 132.17 g, 65percent. NMR and GCMS data are consistent with the required structure., 12150-46-8
As the paragraph descriping shows that 12150-46-8 is playing an increasingly important role.
Reference£º
Patent; Merck Patent GmbH; US2008/217605; (2008); A1;,
Phosphine ligand
Chiral phosphine ligands in asymmetric synthesis. Molecular structure and absolute configuration of (1,5-cyclooctadiene)-(2S,3S)-2,3-bis(diphenylphosphino)butanerhodium(I) perchlorate tetrahydrofuran solvate