29949-84-6, The synthetic route of 29949-84-6 has been constantly updated, and we look forward to future research findings.
29949-84-6, Tris(3-methoxyphenyl)phosphine is a chiral-phosphine-ligands compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated
EXAMPLE 81 7-(3Methoxyphenyl)-1-(4-methylpiperazin-1-yl)naphthalene A mixture of 3-methoxy-1-bromobenzene (0.089 ml, 0.71 mmol), 7-trimethylstannyl-1-(4-methylpiperazin-1-yl)naphthalene (0.25 g, 0.64 mmol), bis-(acetonitrile) palladium chloride (0.0085 g, 0.032 mmol), tri(3-methoxyphenyl)phosphine (0.023 g, 0.064 mmol), and butylated hydroxytoluene (BHT, about 0.001 g, antioxidant) in dimethyl formamide (12 mL) was warned to 110 C. for 2 hours. The reaction was cooled to room temperature and diluted with 1 N aqueous lithium chloride (25 mL) and 1 N sodium hydroxide (2 mL); then extracted with ether (3*). The combined ether layer was washed with 1 N aqueous lithium chloride and brine. The organic phase was dried over calcium sulfate and concentrated. The residue was purified by flash chromatography on silica gel (1*2.5 inches). Elution proceeded as follows: 75% ethyl acetate/hexane, 200 mL, nil; 2% methanol/ethyl acetate 200 mL and 10% methanol/ethyl acetate, 200 mL, 0.084 g of an oil. This oil was further purified by kugelrohr distillation (1 mm Hg). The distillation proceeded as follows: 110-130 C., 0.014 g of a mixture of the title product and 7-methyl-1-(4-methylpiperazin-1-yl)naphthalene: 200-220 C. 0.062 g (23%) of the title compound as a yellow oil: 1H NMR delta 8.43 (incompletely resolved dd, J=1.2Hz, 1 h), 7.90 (d, J=9 Hz, 1 H), 7.74 (dd, J=2,8.5 Hz, 1 H), 7.58 (d, J=8 Hz, 1 H), 7.43 (sym m, 2 H), 7.34 (dt, J=1.5, 7.5 Hz, 1 H), 7.29 (5, J=2 Hz, 1 H), 7.14 (dd, J=1, 7.5 Hz, 1 H), 6.96 (ddd, J=1, 2.5,8 Hz, 1H), 3.92 (s, 3 H) 3.20 (br s, 4 H), 2.75 (br s, 4 H), 2.44 (s, 3 H). The product was dissolved in chloroform and HCL gas was bubbled through the solution to form the hydrochloride salt. Concentration of this solution to about 1 mL. at the boil and addition of about 1 mL of ether caused the white crystalline product to precipitate. The hydrochloride salt weighted 0.057 g: mp 236-238 C. Analysis calculated for C22H24N2O¡¤HCl: C, 71.63; H, 6.83; N, 7.59. Found: C, 71.31; H, 6.92; N, 7.59.
29949-84-6, The synthetic route of 29949-84-6 has been constantly updated, and we look forward to future research findings.
Reference£º
Patent; Chenard, Bertrand L.; Macor, John E.; Segelstein, Barbara E.; US2001/4669; (2001); 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