Reference of 609-12-1,Some common heterocyclic compound, 609-12-1, name is Ethyl 2-bromo-3-methylbutanoate, molecular formula is C7H13BrO2, 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.
52.4 g of activated zinc powder and 450 ml of anhydrous THF,Add a few drops under N2 protectionEthyl alpha-bromoisovalerate2 to trigger the reaction,66 reflux 45min stirring until the reaction liquid becomes dark green after adding 20.324g (0.165mol)Cyclohexyl acetonitrile,And slowly add 2 (88.71 g, 0.4243 mol) within 1 h,Continue to reflow 1H stop heating, cooled to room temperature,Add 80ml 50% K2CO3 solution was stirred vigorously for 10min, the reaction solution was allowed to stratification, the organic phase was separated, the residue was extracted with THF,The combined organic phases were hydrolyzed by adding 150 ml of 15% HCl, the organic layer was separated and concentrated under reduced pressure, the aqueous layer was extracted three times with ethyl acetate,The combined organic phases were washed three times with saturated sodium bicarbonate solution, saturated NaCl, dried over anhydrous Na2SO4,The solvent was removed under reduced pressure to give compound 3 as a crude reddish brown liquid, 38.4 g, which was used directly in the next reaction without purification.
The synthetic route of 609-12-1 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; Yunnan University; Chinese Academy Of Sciences Kunming Animal Institute; He Yanping; Zheng Yongtang; Zhang Yufang; Xiang Siying; Zhang Hongbin; Zhao Zhidong; Yang Liumeng; (9 pag.)CN106866548; (2017); A;,
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