Synthetic Route of 51839-15-7, These common heterocyclic compound, 51839-15-7, name is Dimethyl 5-iodoisophthalate, 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.
Intermediate LXII: Dimethyl-5-trifluoromethyl isophthalate; To a solution of dimethyl 5-iodoisophthalate (1 g, 3.12 mmol) in 1:1 DMF/HMPA was added Methyl- 2,2-difluoro-2( fluorosulfonyl) acetate (3 g, 15.6 mmol) and Copper (I) Iodide (2.9 mg, 15.6 mmol) and the reaction mixture heated to. 80 C for 16 h. The reaction was cooled to rt and diluted with ethyl acetate (200 mL) The solvent was decanted and the copper salts washed with an additional 100 mL of ethyl acetate. The organics were poured into water (200 mL ) the phases separated and the aqueous extracted with Ethyl acetate ( 100mL) dried over anhydrous sodium sulfate, filtered and concentrated at reduced pressure. The residue was chromatographed on silica gel eluting with dichloromethane. to give dimethyl-5-trifluoromethyl isophthalate. : :?H NMR (400 MHz, CDC13) No. 8.85 (s, 1H), 8.48 (s, 2H), 4.01 (s, 6H). LCMS [(M) +H]+ = 263.
The synthetic route of 51839-15-7 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; MERCK & CO., INC.; WO2005/103020; (2005); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com