Related Products of 461432-23-5, These common heterocyclic compound, 461432-23-5, name is 4-Bromo-1-chloro-2-(4-ethoxybenzyl)benzene, 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.
Under nitrogen, to a 50mL three-necked flask were added sequentially 3.99g2- chloro-5-bromo-ethoxy -4`- – diphenylmethane, 10ml of tetrahydrofuran and 30ml of toluene, followed by stirring to dissolve, cooled to -78 deg.] C, was added dropwise 2.4M n-hexane solution of n-butyllithium in 5.48ml, dropping the temperature was kept below -70 deg.] C, after the addition was complete the reaction was complete to give 2-chloro-5-ethoxy-lithium -4`- – diphenyl methane solution. Under nitrogen atmosphere, into a three-necked 250mL flask was added 8.43g Compound B-2 and 40ml of toluene, followed by stirring to dissolve, cooled to -78 deg.] C, the lithium-chloro-5-ethoxy -4`- – diphenylmethane was added dropwise, the dropping rate to keep the temperature below -65 deg.] C, after the addition was complete the reaction was kept 2 hours, 17.63g of tetrabutyl ammonium fluoride was added dropwise, the reaction was stirred for 1 hour at room temperature, methanol was added dropwise a solution of 7.45g of sulfuric acid ( containing 2.56 g of sulfuric acid), after the completion of the dropwise addition, the reaction mixture was stirred at room temperature, the HPLC monitoring of the reaction is complete, add saturated NaHCO3 solution to a pH of about 7.5, the organic layer was separated and the aqueous layer extracted with ethyl acetate, the combined organic phases were washed with saturated brine washed with water, vacuum distillation, additional 20ml toluene, evaporated under reduced pressure rotary evaporation to give 4.16g of intermediate -1, yield: 77.3%.
Statistics shows that 4-Bromo-1-chloro-2-(4-ethoxybenzyl)benzene is playing an increasingly important role. we look forward to future research findings about 461432-23-5.
Reference:
Patent; Beijing Wan-sheng Pharmaceutical Co., Ltd.; Lin, Guoliang; Li, Xiaopeng; Liu, Zhidong; Wang, Zhanwei; Li, Yong; Pei, Yingzi; (15 pag.)CN105481915; (2016); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics