Related Products of 133232-56-1, These common heterocyclic compound, 133232-56-1, name is 3-Iodo-2-methylbenzoic acid, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.
[0469] To a solution of 3-iodo-2-methylbenzoic acid (2.0 g, 3.82 mmol) in dry MeOH (10 mL) at 0 C was added thionyl chloride (681mg, 5.72 mmol). Then the reaction was heated to 80 C for 16 hrs. TLC showed the starting material was consumed and one main spot was present. The reaction was cooled to rt and the solvent was removed. The residue was diluted with water (20 mL) and extracted with EA (40 mL) twice. The combined organic layers were washed with saturated sodium bicarbonate aqueous (30 mL), brine, dried over sodium sulfate, filtered and concentrated providing crude product, which was purified by column chromatography on silica-gel elution with petroleum ether:EA (from 0% to 8%) providing methyl 3-iodo-2-methylbenzoate (1.7 g, 80.4% yield) as a colorless oil. MS (ESI) m/z 277.0 [M+H]+. 1H NMR (400 MHz, CDCl3) delta 7.97 (dd, J = 1.2, 8.0 Hz, 1 H), 7.73 (dd, J = 0.8, 8.0 Hz, 1 H), 6.92 (t, J = 8.0 Hz, 1 H), 3.89 (s, 3 H), 2.66 (s, 3 H).
The synthetic route of 133232-56-1 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; BIOTHERYX, INC.; CHAN, Kyle, W.H.; FUNG, Leah; SULLIVAN, Robert; ERDMAN, Paul, E.; MERCURIO, Frank; (225 pag.)WO2017/201069; (2017); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com