With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.146960-90-9,1,1′-Bis(dicyclohexylphosphino)ferrocene,as a common compound, the synthetic route is as follows.
Example 21 Preparation of[DCyPFc RuCI2AMPY] Into a 200 mL stirred glass reactor are introduced 3.2 g of RuCI2(PPh3)3and 2.32 g of DCyPFc as solids followed by 100 mL of nitrogen saturated MEK. Stirring is started immediately and the slurry is stirred for 28 hours.3P{ H} NMR analysis of a NMR sample obtained by diluting a sample from the reaction mixture with C6D6shows that all DCyPFc has reacted and that the only free phosphine is PPh3released from RuCI2(PPh3)3.To the intermediate slurried in MEK is added 0.42 g of AMPY after dilution in 10 ml of MEK over the period of 10 minutes. The reaction mixture is stirred for 60 hours. The obtained thick slurry of a tan brown product is suction filtered using a Buechner funnel and filter paper until a wet cake of product is obtained. Washing with MEK is continued until the MEK filtrate is uncoloured. The yellow product is dried at 10 mbar, 30C for 48 hours. A sample was slurried in IPA and again filtered.The identity of the solid is confirmed by a combination of H and3P{ H} NMR analysis. By3P{ H} NMR analysis 2 isomers with delta = 51 ppm (major broad resonance) and delta = 48 ppm (minor broad resonance) are visible. The AMPY resonances for the major complex are delta = 9.94 (d), 7.73 (t), 7.40 (t), 7.35 (t) (all integration as 0.75 H) 5.07 (s, 1 .5 H), the AMPY resonances for the minor complex are delta = 9.80 (d), 8.06 (t), 7.93 (t), 7.64 (t) (all integration as 0.25 H), 5.01 (s, 0.5 H). The 2 x 4 CH resonances of ferrocene are at delta = 4.23 (m), 4.08 (m). The remaining resonances of the cyclohexyl – resonances (44) are a broad series of multiplets at delta = 2.2 – 0.94 ppm., 146960-90-9
The synthetic route of 146960-90-9 has been constantly updated, and we look forward to future research findings.
Reference£º
Patent; JOHNSON MATTHEY PUBLIC LIMITED COMPANY; FACCHETTI, Sarah; NEDDEN, Hans; WO2015/79207; (2015); A2;,
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