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. 329944-72-1, name is 3-Bromo-5-chlorotoluene, A new synthetic method of this compound is introduced below., category: chlorides-buliding-blocks
Under a nitrogen atmosphere, a 5 L dry and clean four-neck round bottom flask was charged with diisopropylamine (72.8 g, 0.72 mol, 1.06 eq) and 1500 mL of anhydrous tetrahydrofuran, and the temperature was reduced to -70 C.Add n-butyllithium solution (272mL, 2.5M, 0.68mol, 1.0eq), and reduce the temperature to -70 with stirring.Slowly add D-2 (139g, 0.68mol, 1.0eq) and maintain the reaction for 1h after the addition.Slowly add iodine-tetrahydrofuran solution (172g iodine / 300ml THF, 0.68mol, 1.0eq),After the addition, the reaction was maintained for 1 h.The temperature was slowly raised to room temperature, and the reaction was monitored by HPLC for completion.The reaction was quenched with 500 mL of 5% Na2S2O3 solution, and extracted with 2 L of methyl tert-butyl ether. The organic phase was washed with 1500 mL of saturated brine, dried over anhydrous sodium sulfate, concentrated under reduced pressure to obtain an oil, and recrystallized by adding 650 mL of ethanol.182 g (F-2) of white flake solid was obtained,Yield was 81%.
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; Ningbo Lumilan New Materials Co., Ltd.; Ningbo Dinghao Optoelectric Materials Technology Co., Ltd.; Zhang Yuxiang; Zhang Qingyun; Ding Huanda; Chen Zhikuan; (41 pag.)CN110551154; (2019); A;,
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