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. 65515-28-8, name is Methyl 2,6-dichloronicotinate, the common compound, a new synthetic route is introduced below. Product Details of 65515-28-8
A solution of 4-chlorophenol (12.2 g, 0.095 mol) in 36.6 mL of DMF was added at room temperature to the above solution (19.6 g of ester 2, 0.095 mol), followed by addition of triethylamine (17.3 mL, 0.124 mol) at 20-22 0C over 15 min. Solid DABCO (1.6 g, 14.2 mmol) was added to the resulting solution in one portion. A temperature increase of ~3 0C was observed. A water bath was used to maintain the reaction temperature. The reaction was stirred at 22-24 0C for 4-5 h while monitoring by LC until all of the 4- chlorophenol was consumed, resulting in a light slurry. AcOH (2.72 mL, 47.5 mmol) and IPA (57.5 mL) were added to the light slurry, followed by cold water (30 mL) to maintain the internal temperature at 20-25 0C. When the water was added, a clear solution first formed, and then a slurry of product formed. After stirring at RT for 0.5 h, additional water (86 mL) was added over 0.5 h. After the slurry was stirred at RT for 1-2 h, it was filtered. The filter cake was washed with mixed solvents (60 mL OfIPAiH2O = 1:1). The isolated solid was dried in a vacuum-oven at 50 0C for 8 h to provide the product as white cotton-like solid.
The synthetic route of 65515-28-8 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; MERCK & CO., INC.; WO2006/96564; (2006); A1;,
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