Electric Literature of 13101-40-1, 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 13101-40-1 as follows.
Nitrogen was passed into the three-necked flask equipped with mechanical stirring, thermometer and condenser,Add 100.0 mL of toluene, compound 5b-4 (20 mmol),Starting material 3-chloro-5-bromoiodobenzene (ie compound 5b-5, 21 mmol),Potassium carbonate (40 mmol), 20 mL ethanol, 20 mL water. Start stirring,The temperature was raised to 50 C, and tetrakistriphenylphosphine palladium (0.2 mmol) was quickly added.Continue heating to reflux state for 6h, pour into 100mL water with stirring,After standing, the liquid was separated, and the aqueous phase was extracted with 50 mL of toluene, and the organic phases were combined.Dry with 10g of anhydrous sodium sulfate, filter, and concentrate the filtrate (70 , -0.09MPa),Concentrate to distill off without solvent, add 50ml n-heptane,Filtration gave compound 5b-6 (17 mmol) in 85% yield.
According to the analysis of related databases, 13101-40-1, the application of this compound in the production field has become more and more popular.
Reference:
Patent; Shanxi Laite Optoelectric Materials Co., Ltd.; Wang Jinping; Xue Zhen; Chen Zhiwei; (47 pag.)CN110981860; (2020); A;,
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