Reference of 694-48-4, These common heterocyclic compound, 694-48-4, name is 1,3-Dimethyl-1H-pyrazole, 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.
Put 100g (1.04mol, 1eq) of 1,3-dimethylpyrazole into the reaction bottleAnd 800mL water and 400mL ethanol,Add in batches with stirring at room temperature132.1g (0.52mol, 0.5eq) of iodine,Subsequently, 84.8 g (0.624 mol, 0.6 eq) of 25% hydrogen peroxide was added dropwise at 15-20C.Stir at room temperature for 20 hours,Sampling GC to check the remaining material is less than 1%, add 200mL of saturated sodium bisulfite,Distilling ethanol under reduced pressure, cooling to 0, filteringget210.1g of 4-iodine-1,3-dimethyl-1H-pyrazole, GC purity 98.6%,The yield was 91%.
Statistics shows that 1,3-Dimethyl-1H-pyrazole is playing an increasingly important role. we look forward to future research findings about 694-48-4.
Reference:
Patent; Xuzhou Shengyuan Chemical Co., Ltd.; Chen Hong; Yu Wanli; (8 pag.)CN111233768; (2020); A;,
Pyrazole – Wikipedia,
Pyrazoles – an overview | ScienceDirect Topics