Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 6698-13-1, name is 4-Bromo-1,3-benzodioxole, A new synthetic method of this compound is introduced below., Quality Control of 4-Bromo-1,3-benzodioxole
The compound 4-bromobenzo[d][1,3]dioxole (5g, 24.873mmol)And sublimation sulfur (0.848g, 26.2mmol) was added to the two-necked flask, under the protection of nitrogen, was added tetrahydrofuran (100mL), cooled to -70 and stirred for 30 minutes,Slowly add hexane solution of tert-butyllithium (38mL, 49mmol, 1.3mol/L),After the dropwise addition, the reaction was continued at this temperature for 2 hours,Saturated ammonium chloride solution (100 mL) was added dropwise to quench the reaction, ethyl acetate (200 mL) was added for extraction, liquid separation, the organic phase was washed with 2N sodium hydroxide solution (20 mL), and the aqueous phases were combined,After adjusting the pH of the aqueous phase to about 4-5 with 4N hydrochloric acid, extract the aqueous phase with ethyl acetate (100 mL×2),The organic phases were combined, and the organic phase was washed with saturated sodium chloride solution (100 mL), dried over anhydrous sodium sulfate, and filtered.The filtrate was concentrated under reduced pressure to give the title compound as a yellow oil (3.12g, 81.4%).
The synthetic route of 6698-13-1 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; Guangdong Dongyangguang Pharmaceutical Co., Ltd.; Luo Huichao; Ren Qingyun; Yin Junjun; Wu Chunlin; Fan Yuxin; Mo Yufeng; Zhang Yingjun; (102 pag.)CN111057074; (2020); A;,
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