In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 69518-17-8, name is 4-Iodophthalonitrile belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Quality Control of 4-Iodophthalonitrile
EXAMPLE 71 (1S,2R)-4′-(2-Hydroxy-1-methyl-4-pyridin-3-ylbutoxy)biphenyl-3,4-dicarbonitrile Prepared according to the method described in Example 12b) from (1S,2R)-4-(2-hydroxy-1-methyl-4-pyridin-3-ylbutoxy)benzeneboronic acid (0.197 g, Example 33), 4-iodo-1,2-dicyanobenzene (0.421 g, Can. J. Chem., 1985, 63, 3057), 2M aqueous sodium carbonate (0.50 ml) and tetrakis(triphenylphosphine)palladium (0) (0.054 g) in ethanol (3 ml). The reaction mixture was heated in a sealed vial at 90 C. for 4 hours. After cooling, the solution was concentrated under reduced pressure and the residue purified by chromatography over silica eluding with ethyl acetate. The residue was further purified by chromatography over silica gel eluding with dichloromethane:2-propanol (19:1). The residue was then further purified by reverse-phase HPLC eluding a gradient of 25-100% acetonitrile in 0.1 w/v aqueous ammonium acetate solution. The HPLC fractions were concentrated under reduced pressure, the residue dissolved in dichloromethane, filtered and concentrated under reduced pressure. The residue was triturated with ether to give the title to compound as a solid (0.060 g). m.p. 135.5-137 C. MS (APCI) 384 (M+H)+ 1H NMR (DMSO) 8.47-8.43(2H, m); 8.38(1H, dd); 8.25-8.12(2H, m); 7.79(2H, d), 7.63(1H, dt); 7.30(1H, dd); 7.06(2H, d); 5.03(1H, d); 4.41(1H, quintet); 3.63-3.5(1H, m); 2.9-2.75(1H, m); 2.75-2.6(1H, m); 1.95-1.8(1H, m); 1.75-1.55(1H, m); 1.24(3H, d).
The synthetic route of 69518-17-8 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; AstraZeneca AB; US6300352; (2001); B1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com