Reference of 52807-27-9,Some common heterocyclic compound, 52807-27-9, name is 4-Chloro-2-iodoanisole, molecular formula is C7H6ClIO, 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.
4-Chloro-2-iodophenol; 109.4g (0.436mol) of boron tribromide were added over 10 minutes to a stirred solution of 9Og (0.335mol) of 4-chloro-2-iodoanisole in dichloromethane (900ml) at -780C under nitrogen. Cooling was removed and allowed to warm to room temperature and stirred for 5 hours. Poured onto ice and diluted with a further 800ml of water. The organic phase was separated, the aqueous extracted with dichloromethane and the combined organics washed with saturated sodium bicarbonate, dried and evaporated to give 84.87g of off- white solid; Sodium 6-r(5-chloro-2-fr(4-chloro-2-fluorophenyl)methvnoxy)phenyl)methvn-2- pyridinecarboxylate (Alternative route 2); 4-Chloro-2-iodophenol; Boron tribromide (1349g) was added to a solution of 4-chloro-2-iodoanisole (1025g) in dichloromethane (10.3L) under nitrogen at such a rate that the temperature remained at 0- 5C The solution was then warmed to 200C and stirred for c. 19h until the reaction was complete by HPLC. This organic solution was added to water (8.2L) and the mixture was cooled to 5C to 10C. DCM (770ml) was added and the resuting biphasic mixture was then stirred at 50C for 15 min before being warmed to 220C and then finally stirred at 22C for 20 min before separating the phases. The separated organic phase was washed with aqueous saturated sodium bicarbonate (3.1L), water (3.1L) and then evaporated on a Buchi to give the title compound. (963.6g)
The synthetic route of 52807-27-9 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; GLAXO GROUP LIMITED; WO2006/66968; (2006); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com