With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.24171-89-9,Tri(thiophen-2-yl)phosphine,as a common compound, the synthetic route is as follows.
A benzene solution (20 mL) of 1 (30 mg, 0.054 mmol) and PTh3 (15 mg, 0.054 mmol) was refluxed for 12 h. The solvent was removed under reduced pressure and the residue chromatographed by TLC on silica gel. Elution with cyclohexane/CH2Cl2 (9:1, v/v) developed three bands. The faster band was unreacted 1 (6 mg), while the second band afforded [Fe2(CO)5(PTh3)(mu-Th)(mu-PTh2)] (2b) (12 mg, 27%) as an orange powder. Spectroscopic data for this band before crystallization showed the presence of a second complex (ca. 10%) that was assigned as [Fe2(CO)5(PTh3)(mu-O=C-Th)(mu-PTh2)] (3b). Recrystallization of the mixture from hexane/CH2Cl2 at 4C gave a crystalline product from which a crystal of [Fe2(CO)5(PTh3)(mu-O=C-Th)(mu-PTh2)] (3b) was selected for crystallography. The third band gave a small amount (ca. 2 mg) of a yellow solid, tentatively identified as [Fe2(CO)6(PTh3)(eta1-Th)(mu-PTh2)]. Spectral data: IR(m(CO), CH2Cl2): 2059 vs, 2018 vs, 1998 s, 1975 w, 1958 br and1895 w. 1H NMR (CDCl3): d 7.88 (d, J 2, 1H), 7.77 (s, 2H), 7.62 (d,J 6, 3H), 7.53 (br, 1H), 7.35 (s, 3H), 7.10 (s, 3H), 6.95 (br, 2H) 6.76(br, 1H), 6.55 (br, 1H), 6.17 (br, 1H). 31P{1H} NMR (CDCl3): d137.0 (d, J 48, P), 40.0 (d, J 48, 1P). Spectral data for 2b: Anal.Calc. for C29H18Fe2O5P2S6: C, 42.87; H, 2.23%. Found: C, 42.91; H,2.25%. IR (m(CO), CH2Cl2): 2038 vs, 1990 s, 1977 sh and 1948 wcm1 1H NMR (CDCl3): d 7.64 (d, J 2.0, 1H), 7.57 (m, 4H), 7.42 (d,J 2.0, 1H), 7.22 (m, 3H), 7.09 (m, 5H), 6.75 (t, J 4.0, 1H) 6.63 (t, J4.0, 1H), 6.37 (m, 1H), 4.79 (d, J 2.0, 1H). 31P{1H} NMR (CDCl3): d92.3 (d, J 24, 1P), 35.0 (d, J 24, 1P). Spectral data for 3b: IR(m(CO), CH2Cl2): 2036 vs, 1981 s, 1952 w and 1934 w cm1.31P{1H} NMR (CDCl3): d 71.7 (d, J 100, 1P), 33.2 (d, J 100, 1P)., 24171-89-9
As the paragraph descriping shows that 24171-89-9 is playing an increasingly important role.
Reference£º
Article; Rahaman, Ahibur; Alam, Fakir Rafiqul; Hossain, Md. Kamal; Abdel-Magied, Ahmed F.; Ghosh, Shishir; Tocher, Derek A.; Haukka, Matti; Kabir, Shariff E.; Nordlander, Ebbe; Hogarth, Graeme; Inorganica Chimica Acta; vol. 430; (2015); p. 208 – 215;,
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