In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 461432-23-5, name is 4-Bromo-1-chloro-2-(4-ethoxybenzyl)benzene belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. HPLC of Formula: C15H14BrClO
A mixture of 4-bromo-1-chloro-2-(4-ethoxybenzyl)benzene compound of formula-4 (83.33 gms) and toluene (420 ml) was heated to reflux temperature and stirred for 2 hrs under azeotropic conditions. Distilled off the solvent completely under reduced pressure. Cooled the obtained compound to 25-30 C. under nitrogen atmosphere. Tetrahydrofuran (665 ml) followed by the compound obtained in step-(a) were added to the reaction mixture at 25-30 C. under nitrogen atmosphere. Cooled the reaction mixture to -85 to -80 C. and stirred for 20 mins at the same temperature. n-butyl lithium (238.3 ml) was slowly added to the reaction mixture at -85 to -80 C. under nitrogen atmosphere. Raised the temperature of the reaction mixture to -75 to -70 C. and stirred for 2 hrs at the same temperature. A solution of methane sulfonic acid (91.4 ml) in methanol (500 ml) was slowly added to the reaction mixture at -75 to -70 C. The temperature of the reaction mixture was slowly raised to 0-5 C. and then to 10-15 C. The reaction mixture was stirred for 18 hrs at 10-15 C. 10% aqueous sodium bicarbonate solution was added to the reaction mixture at 10-15 C. The temperature of the reaction mixture was raised to 25-30 C. and stirred for 15 mins. Separated the both organic and aqueous layers, the aqueous layer was extracted with ethyl acetate. Both the organic layers were combined, washed with 10% aqueous sodium chloride solution and then distilled off the solvent completely from the organic layer under reduced pressure. Cooled the obtained compound to 40-45 C. and then co-distilled with toluene. Toluene (100 ml) was added to the obtained compound at 25-30 C. and stirred for 20 mins at the same temperature. Diisopropyl ether (500 ml) was added to the reaction mixture at 25-30 C. Cooled the reaction mixture to 15-20 C. and stirred for 2 hrs at the same temperature. Settled the reaction mixture and decanted the upper organic layer. Distilled off the solvent from the bottom to get title compound. Yield: 135 gms; Purity by HPLC: 89.02%.
The synthetic route of 461432-23-5 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; MSN LABORATORIES PRIVATE LIMITED; Thirumalai Rajan, Srinivasan; Eswaraiah, Sajja; (15 pag.)US2017/29398; (2017); A1;,
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