With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.148332-36-9,[2,2′:6′,2”-Terpyridine]-4′-carboxylic acid,as a common compound, the synthetic route is as follows.
General procedure: Typically, 2-(4-carboxyphenyl)-4,6-dipyrid-2-yltriazine (1.0 g,2.81 mmol) was heated to reflux in thionyl chloride (30 mL) for0.5 h, after which no solid suspension remained. The excess thionylchloride was removed by distillation and the residue was driedunder vacuum, dry methanol (60 mL) was added and the reactionmixture was heated to reflux until no solid suspension remained(2 h). The solution was cooled to room temperature and addedto H2O (300 mL) forming a voluminous precipitate of the methylester ligand which was isolated by filtration and dried in vacuowithout further purification. Typically, the ligand (0.25 g,0.68 mmol) was heated to reflux in DMF with RuCl3 (0.07 g,0.34 mmol) and AgNO3 (0.173 g, 1.02 mmol) after which the solutionwas filtered to remove AgCl(s). The filtrate was then decantedinto a solution of NH4PF6 (aq) (300 mL), and the resultant heavyprecipitate was isolated by filtration and washed with water, thendissolved in a minimal amount of acetonitrile for chromatographicpurification using silica and a 7:2 CH3CN/KNO3 (aq, sat) mixture aseluent. The collected fractions are combined, and to this addedNH4PF6 and enough DCM to effect a phase separation. After washingthe organic phase, the aqueous phase was discarded and theprocess repeated, with a final washing with water alone. Theorganic phase was dried and the residue taken up in a minimalamount of acetonitrile, then poured into H2O (300 mL) to give aheavy precipitate which was filtered and dried in vacuo. Yield:0.263 g (69percent), Rf = 0.55 (silica, 7:2 CH3CN/KNO3 (sat, aq) as eluent).1H NMR (400 MHz, CD3CN) d ppm 9.19 (d, J = 8.4 Hz, 4H), 9.14 (d,J = 7.7 Hz, 4H), 8.44 (d, J = 8.4 Hz, 4H), 8.16 (m, 4H), 7.73 (d,J = 5.3 Hz, 4H), 7.41 (m, 4H), 4.02 (s, 3H). ESI-MS: [M]2+ Cald. forC42H30N10O4Ru: 420.07475. Found: 420.07499.
148332-36-9, As the paragraph descriping shows that 148332-36-9 is playing an increasingly important role.
Reference£º
Article; Cooke, Michael W.; Santoni, Marie-Pierre; Loiseau, Frederique; Hasenknopf, Bernold; Hanan, Garry S.; Inorganica Chimica Acta; vol. 454; (2017); p. 208 – 215;,
Metal catalyst and ligand design
Ligand Template Strategies for Catalyst Encapsulation – NCBI