Reference of 5332-26-3, These common heterocyclic compound, 5332-26-3, name is 2-(Bromomethyl)isoindoline-1,3-dione, 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.
Weigh Intermediate LNa-3 (0.1g, 0.4984mmol) in 50mL round-bottom flask was added dimethyl formamide (15mL) was dissolved with stirring at room temperature, was added sodium bicarbonate (0.0460g, 0.5482mmol) was stirred heated to 40 after 1.5h, then slowly added dropwise bromomethyl-N- phthalimide (0.2393g, 0.9968mmol) in dimethyl formamide dropwise completed (2h), TLC monitoring, the reaction is complete, the reaction is stopped, most of the solvent was distilled off, ethyl acetate (6mL) reconstituted added washed three times (3 ¡Á 5mL), saturated brine (5mL) wash, dried over anhydrous sodium sulfate, filtered, and the filtrate evaporated to dryness to give the crude product, and then with the volume fraction of 95% ethanol recrystallization, in pure LN-S-5.In various intermediate and LN-3-bromomethyl-N- phthalimide were prepared by the above process the compound LN-S-5 ~ target product LN-S-8, the results are as follows:
The synthetic route of 5332-26-3 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; Shandong University; Liu, Xinyong; Liu, Na; Zhan, Peng; Jia, Haiyong; (24 pag.)CN106008506; (2016); A;,
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