In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 33070-32-5 as follows. HPLC of Formula: C7H3BrF2O2
Magnesium turnings (11.12g, 0.464mol) and anhydrous tetrahydrofuran (600 ml) were placed in a round-bottomed flask fitted with a mechanical stirrer, reflux condenser, pressure equalizing addition funnel and drying tube. 5-Bromo-2,2- difluoro-l,3-benzodioxole (lOOg) was added to the flask under nitrogen atmosphere. The temperature of the reaction mass was raised to 40C during initiation. Upon initiation, remaining 5-Bromo-2,2-difluoro-l,3-benzodioxole (lOOg) was added drop- wise to the reaction mass. The temperature of the reaction mass was maintained below 40C. The progress of the reaction was monitored by gas chromatography. The reaction mass was then cooled to 0C and carbon-dioxide gas was passed for 2 hours at 0C. The raction was monitored by liquid chromatography for completion. The reaction mass was quenched with 10% HC1 (230g). The organic layer was separated, concentrated to obtain solid. The solid was washed with water (50g) and dichloromethane (50g), filtered and dried at 60C under 50mmHg for 2 hours to obtain the title compound. Yield (%): 70 Purity (%): 99 (by liquid chromatography)
According to the analysis of related databases, 33070-32-5, the application of this compound in the production field has become more and more popular.
Reference:
Patent; SRF LIMITED; KUMARASAMY, Radha; RAJARAM, Aiyswariya; GANESAN, Varadharaj; RAVICHANDRAN, Poornachandran; BOKKA, Deepak; KAVERIKKANNAN, Nagarajan; BASHA, Thurabudin Mohamed Kaleel; SEETHARAMAN, Prasannakumar; MARI, Chandra Mohan; KUMAR, Kapil; ANAND, Rajdeep; (15 pag.)WO2017/46816; (2017); A2;,
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