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. 10016-52-1, name is 2,8-Dibromodibenzo[b,d]furan, A new synthetic method of this compound is introduced below., 10016-52-1
A single-mouth flask was taken, 3.26 g of 3,6-dibromodibenzothiophene was added, sealed and vacuum-dried with nitrogen three times, and 100 mL of anhydrous tetrahydrofuran (THF) was dissolved and dissolved under a nitrogen atmosphere.The device was then placed in a dry ice/acetone bath at -78 C for 15 min.13.75 mL of a n-hexane solution of n-butyllithium was weighed using a syringe.The mixture was added dropwise to a reaction flask, and reacted at -78 C for 1.5 h under a nitrogen atmosphere to obtain a reaction system.3.74 mL of diphenylphosphonium chloride was added to the reaction system, and the mixture was allowed to react at room temperature for 12 hours.The reaction solution was quenched with 50 mL of water and extracted with 3¡Á50 mL of dichloromethane.The organic phase was collected and dried over anhydrous sodium sulfate. The dichloromethane solution was spun off using a rotary evaporator.The crude product was then dissolved in 50 mL of dichloromethane, silica gel powder was added and the solvent was dried.Purification by chromatography gave an arylphosphine derivative. The obtained arylphosphine derivative and 0.6 gThe sulfur powder was dissolved in a dichloromethane solution and allowed to react at room temperature overnight.The dichloromethane solution was spun off using a rotary evaporator. Then the crude product was dissolved to 50 mLAdd silica gel to the dichloromethane and spin dry the solvent.Purification by chromatography gave 1.91 g of a white solid.The yield was 37.1%.
The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.
Reference:
Patent; Nanjing University of Posts and Telecommunications; Tao Ye; Li Huanhuan; Jiang Yunbo; Zhi Yibin; Chen Runfeng; Huang Wei; (11 pag.)CN109912654; (2019); A;,
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