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.
Dimethyl-5-iodoisophthalate (1.35 g, 4.21 mmol, Matrix Scientific, Columbia, SC) and lithium hydroxide monohydrate (884 mg, 20.07 mmol) were taken in a mixture of 3.95 mL methanol and 0.99 mL water and the suspension was stirred vigorously at 20 C for 3.5 h. The mixture was diluted with aqueous saturated sodium bicarbonate to a volume of 75 mL, and unreacted ester was removed by extraction with 75 mL ethyl acetate. The aqueous layer was carefully acidified with 1 M HCl to pH 2 and the resultant acid was extracted twice with 250 mL ethyl acetate. The ethyl acetate fractions were combined, dried over sodium sulfate, and the ethyl acetate was evaporated to give a white powder (965 mg, 78.4%): mp 302-303 C 1H NMR-300 MHz (CD3OD) delta 8.55 (d, 2H), 8.60 (d, 1H). 13C NMR (126 MHz, CD3OD) delta 92.6, 129.5, 132.6, 142.2, 165.7. MS (LCMS-ESI; negative ion mode) m/z: 290.7 (M-H)-; HRMS (FAB-) Calcd for C8H4IO4 (M-H)- 290.9154. Found 290.9141 ¡À 0.0000 (n = 2).
The synthetic route of 51839-15-7 has been constantly updated, and we look forward to future research findings.
Reference:
Article; Vaidyanathan; White; Affleck; Zhao; Welsh; McDougald; Choi; Zalutsky; Bioorganic and Medicinal Chemistry; vol. 20; 24; (2012); p. 6929 – 6939;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com