As a common heterocyclic compound, it belongs to copper-catalyst compound, name is Copper(II) sulfate pentahydrate, and cas is 7758-99-8, its synthesis route is as follows.,7758-99-8
18 g of copper sulphate and 6.75 g of sodium bromide were added to 150 ML of D. M water in a 3 necked round bottom flask. The contents of flask were heated to 76-78 C to obtain a clear solution. 6g of sodium metabisulphite was then added to it in portions and stirred for 15 min. The reaction mixture was cooled to 30 2 C. CuBr solid was filtered. To 150 g of compound of formula 2 was added 1.5 1 of acetone and 600 ml of methanol. The contents of the flask were cooled to 18-20 C. 245 ml of aqueous HBR was added to the above reaction mixture at 18-20 C in a single charge. Cool the contents of the flask to 0-2 C. 120ML of 50% w/v aqueous sodium nitrite solution was added slowly to the reaction mixture by maintaining the temperature between 0-2 C, over a period of 30 minutes. The reaction mixture was maintained for 15 minutes at 0-2 C. The temperature was raised to 20-22 C. A solution of 246g of acrylamide in 900ML of acetone was added at 22-23 C in single charge. The reaction mixture was stirred for 10 minutes at 23-24 C, 4. 6g of cuprous bromide was added in a single charge under vigorous stirring and the reaction mixture maintained for 2 hours at 30-35 C. After completion of the reaction, acetone and methanol were. distilled off completely to obtain thick liquid mass. A solution of 150 g of sodium bicarbonate in 3.0 1 of D. M water was prepared. 600ML of hexane was added to it and stirred to get a clear biphasic solution. The reaction mixture was gradually quenched into above flask containing aqueous sodium bicarbonate and hexane solution over a period of 30 minutes at 23-35 C followed by stirring for 2 hours. The product was filtered and the product cake washed with D. M. Water followed by hexane and dried. The crude product obtained was suspended in water and stirred for 1 hour at 25-30 C. The product was filtered and cake washed with D. M. Water followed by hexane. The product thus obtained was suspended in hexane and stirred for 2 hours at 35- 40C. It was filtered and washed with hexane and dried to get compound of formula 3.
With the complex challenges of chemical substances, we look forward to future research findings about 7758-99-8,belong copper-catalyst compound
Reference£º
Patent; SUN PHARMACEUTICAL INDUSTRIES LIMITED; WO2004/108721; (2004); A1;,
Copper catalysis in organic synthesis – NCBI
Special Issue “Fundamentals and Applications of Copper-Based Catalysts”