Adding a certain compound to certain chemical reactions, such as: 13421-13-1, name is 4-Chloro-2-iodobenzoic acid, belongs to iodides-buliding-blocks compound, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 13421-13-1, Recommanded Product: 13421-13-1
4-chloro-2-iodobenzoic acid 7a (15 g, 53 mmol) was dissolved in dry THF (250 mL) and the solution was cooled to 0 C. Hereupon, NEt3 (1 1 mL, 80 mmol) and ethyl chloroformate (7.6 mL, 80 mmol) were added. The reaction was stirred for 1.5 hour and subsequently NaBH (8.0 g, 210 mmol) was added in four portions. After 1.5 hour, additional NaBH (4.0 g, 105 mmol) was added and the reaction was stirred for another hour. Hereupon, the reaction was quenched with H20 (100 mL) and EtOAc (200 mL) was added. The organic layer was washed with H20 (3 chi 150 mL), brine (100 mL) and subsequently dried over MgS04. The solvents were removed under reduced pressure and the crude product was obtained by gradient column chromatography (EtOAc/-heptane, 1 :9 to 1 :6). Compound 8a was obtained as white solid (8.4 g, 75% over 2 steps). 1H-NMR (400 MHz, CDC13) delta: 7.82 (s, 1H), 7.45-7.33 (m, 2H), 4.65 (d, J = 6.2 Hz, 2H), 1.94 (t, J = 6.2 Hz, 1H). 13C- NMR (75 MHz, CDC13) delta: 141.1, 138.3, 133.8, 128.8, 128.6, 96.9, 68.6. HRMS (EI+) m/z calcd for C7H60C1I [M]’+ 267.9152, found 267.9160.
At the same time, in my other blogs, there are other synthetic methods of this type of compound, 4-Chloro-2-iodobenzoic acid, and friends who are interested can also refer to it.
Reference:
Patent; STICHTING KATHOLIEKE UNIVERSITEIT; SYNAFFIX B.V.; DEBETS, Marjoke Froukje; RUTJES, Floris Petrus Johannes Theodorus; VAN HEST, Jan Cornelis Maria; VAN DELFT, Floris Louis; VAN BERKEL, Sander Sebastiaan; WO2014/189370; (2014); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com