Electric Literature of 1875-88-3 , The common heterocyclic compound, 1875-88-3, name is 2-(4-Chlorophenyl)ethanol, molecular formula is C8H9ClO, 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.
The present invention uses SM-A and LCS-1 condensation to prepare Impurity F.Specific operations are as follows: 40g of p-chlorophenylacetic acid was added to 400ml of tetrahydrofuran,Stirring at room temperature dissolved; lithium aluminum hydride in batches, temperature control at 25 ~ 30 ,After the reaction was stirred for 20 hours, 200 ml of water was added slowly and the addition was completed.Add ethyl acetate 400ml stirred 30min, liquid separation, organic phase plus 200ml saturated brine and dried over 20g anhydrous sodium sulfate, filtered, the filtrate was concentrated under reduced pressure 40 ~ 45 ,36.7 g of oil (S2) was obtained; S2 was added to the reaction flask, the temperature was lowered to 0 to 5 C in ice water,Slowly dropping phosphorus tribromide, dropping temperature during the course of 0 ~ 5 , the dropwise addition is completed,Heated to 25 ~ 30 , incubated for 3h,Add water 80ml, stirred 30min, liquid separation, the aqueous phase was extracted with dichloromethane 100ml × 2,The organic phases were combined and concentrated under reduced pressure to give an oil (S3): 48.8 g. Yield: 94.9%.
The synthetic route of 1875-88-3 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; Shandong Kexing Biological Products Co., Ltd.; Cui Ning; Dong Xiangjun; Hao Zhihai; (34 pag.)CN106478506; (2017); A;,
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