Synthetic Route of 773136-66-6, In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 773136-66-6 as follows.
Add NaH (3.71 g, 92.8 mmol, 60.0% purity, 1.3e q) to dry THF (131.0 mL).Compound 2 (21.0 g, 71.4 mmol, 1 eq) and 1-vinylpyrrolidin-2-one (8.49 g, 76.4 mm ol, 8.17 mL, 1.07 eq).The mixture was stirred at 80 C for 3 hours.It was then cooled to room temperature.Then 10% HCl solution (30 mL) was slowly added and stirred at 100 C for 10 hours.The progress of the reaction was detected by TLC (P etroleum ether/Ethyl acetate = 4/1, Rf = 0.68).When the reaction is over,In the condition of an ice bath,Gradually add 1M NaOH solution,The pH of the reaction solution was adjusted to 8.0.Further extraction with DCM (50.0 mL x 2),And by column chromatography (SiO2,Petroleum ether/Ethyl acetate=8/1to 5/1),Obtained white compound 3 (1.60 g, 5.53 mmol,7.75% yield).Figure 4 shows the results of TLC chromatography for this reaction.The NMR data for Compound 3 is:
According to the analysis of related databases, 773136-66-6, the application of this compound in the production field has become more and more popular.
Reference:
Patent; Shanghai Health Medical School; Tang Dewei; Huang Gang; Huang Chen; Wu Xingyu; Yu Meicen; Li Yanjiao; (18 pag.)CN109942582; (2019); A;,
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