With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.14162-94-8,4-Chloro-2,2′-bipyridine,as a common compound, the synthetic route is as follows.
0.303 g (9.45¡Á10-4 mol) of compound 1 and 2 g of KOH were stirred in 10 mL of DMSO for 10 min. 0.645 g (3.38¡Á10-3) of 4-chloro-2,2′-bipyridine was added. The reaction mixture was continuously stirred under argon at 50 C. for 22 hrs. After reaction, the mixture was poured into 30 mL of water. Extraction with 100 mL of CH2Cl2 was tried when the solution was highly alkaline but it was found difficult to separate the two phases. After evaporation of CH2Cl2, the oil was purified by chromatography (silica gel treated with 20% triethylamine in hexane, elution 5-10% methanol in CH2Cl2 and pure methanol) and vacuum dried to afford a sticky transparent product. This was dissolved in methanol and precipitated in acidified water to yield 52 mg of white powder. The remaining water phase was adjusted to pH=8 with NH3H2O. The solution was further extracted with CH2Cl2 until no more bipyridine derivatives could be detected by TLC. After evaporation of CH2Cl2, the oil was purified by chromatography (silica gel treated with 20% triethylamine in hexane, elution 5-10% methanol in CH2Cl2, and pure methanol), vacuum dried and precipitated in acidified water to yield 223 mg of product. The yield for the combined product is 37%. 1H NMR (400 MHz, CDCl3) delta 8.63 (d, 3 H), 8.45 (d, 3H), 8.32 (d, 3 H), 7.4-8.2 (b, 4 H, NH4), 7.97 (d, 3 H), 7.76 (t,3 H), 7.26 (t, 3 H), 6.84 (dd, 3 H), 4.39 (s, 6 H, 3 CH2O), 3.72 (s, 2 H, CH2O), 3.38 (t,2 H, OCH2), 2.20 (t, 2 H, CH2), 1.53 (q, 2 H, CH2), 1.45. (q, 2 H, CH2), 1.0-1.2 (b, 12 H, 6 CH2)., 14162-94-8
14162-94-8 4-Chloro-2,2′-bipyridine 15207243, acatalyst-ligand compound, is more and more widely used in various fields.
Reference£º
Patent; Zhou, Ming; Roovers, Jacques; US2005/59834; (2005); A1;,
Metal catalyst and ligand design
Ligand Template Strategies for Catalyst Encapsulation – NCBI