Technology Process of (1,1,1-tris(diphenylphosphinomethyl)ethane)Ir(H)3
There total 16 articles about (1,1,1-tris(diphenylphosphinomethyl)ethane)Ir(H)3 which
guide to synthetic route it.
The literature collected by LookChem mainly comes from the sharing of users and the free literature resources found by Internet computing technology. We keep the original model of the professional version of literature to make it easier and faster for users to retrieve and use. At the same time, we analyze and calculate the most feasible synthesis route with the highest yield for your reference as below:
synthetic route:
- Guidance literature:
-
In
tetrahydrofuran; diethyl ether;
N2 atmosphere, addn. of excess soln. of LiAlH4 in Et2O to suspension of IrCl3(triphos) in THF, warming (30 min), cooling to room temp., stirring (3 h, laboratory atmosphere); hydrolysis (aq. NaOH), extraction (CH2Cl2), crystn. (CH2Cl2/hexane);
DOI:10.1021/ja00188a027
- Guidance literature:
-
In
tetrahydrofuran;
THF soln. (IrCl(COE)2)2 was treated under N2 with 1 equiv. triphos, after gentle heating to 40°C 10-fold excess LiAlH4 was added in small portions with stirring and slurry was refluxed for 4 h; soln. was cooled to room temp., excess LiAlH4 was hydrolyzed with THF/H2O mixt (1:1, v/v), soln. was filtered and concd. under vac., 1:1 mixt. EtOH/n-hexane was added, soln. was concd. under N2 flow;
DOI:10.1021/ic990667q
- Guidance literature:
-
With
hydrogen;
In
tetrahydrofuran; toluene;
byproducts: benzene, ethane; inert atmosphere; autoclave with Ir-complex evacuation, solvent addn. (suction), H2 addn. up to 2.5 atm, autoclave heating at 150°C for 2 h, mixt. cooling at room temp.; solvent distn. (red. pressure), BPh3 sepn. by sublimation (70°C, 0.5 Torr), Ir-complex identification by NMR and IR spectroscopy;
DOI:10.1021/ja00058a021
