Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 103440-52-4, name is Methyl 2-Iodo-5-methylbenzoate, A new synthetic method of this compound is introduced below., COA of Formula: C9H9IO2
Step (ii); 2-Butoxy-9-(4-iodo-3-methoxycarbonylbenzyl)-8-methoxyadenine; [Show Image] To 4-iodo-3-methoxycarbonyltoluene 1.7 g (6.2mmol) obtained in step (i) in carbon tetrachloride (30ml) were added NBS 1.2g (6.8mmol) and perbenzoic acid 100mg, and the mixture was stirred at 90C for 6.5 hours. After filtration and concentration, to the residue was added water and the mixture was extracted with chloroform. The organic layer was washed with water and saturated brine, dried over Na2SO4 and concentrated. The residue dried in vacuo was dissolved in DMF (30ml). Thereto were added 2-butoxy-8-methoxyadenine, trifluoroacetic acid 1.73g (4.9mmol) and potassium carbonate 1.7g (12.3mmol) and the mixture was stirred at room temperature for 13 hours. After filtration and concentration, to the residue was added water, and the mixture was extracted with chloroform-methanol. The organic layer was washed with water and saturated brine, dried over Na2SO4, and concentrated. The residue was purified by silica gel column chromatography to give the titled compound 620mg (1.2mmol) as a reddish brown oil. Yield 25% 1H NMR (DMSO-d6) delta 7.97 (1H, d, J = 8.2 Hz), 7.64 (1H, brs), 7.10 (1H, d, J = 8.2 Hz), 6.87 (2H, brs), 5.04 (2H, s), 4.15 (2H, t, J = 6.6 Hz), 4.05 (3H, s), 3.83 (3H, s), 1.65-1.61 (2H, m), 1.40-4.35 (2H, m), 0.92 (3H, t, J = 7.4 Hz).
The synthetic route of 103440-52-4 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; Dainippon Sumitomo Pharma Co., Ltd.; AstraZeneca AB; EP1939202; (2008); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com