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. 1996-30-1, name is 3-Bromo-4-fluorochlorobenzene, A new synthetic method of this compound is introduced below., 1996-30-1
Carbazole (800 mmol, 133.8 g), 2-bromo-4-chloro-1-fluorobenzene (840 mmol 175.9 g), and dimethylformamide (160 ml) were added to a three-necked flask, and the flask was flushed with nitrogen. Sodium hydride (62% paraffin dispersion) (800 mmol, 31.0 g) was added thereto stepwise five or more times, while observing the amount of hydrogen gas generated, and the reaction mixture was slowly heated while observing the amount of hydrogen gas generated. The reaction mixture was then heated under stirring at a temperature of 150 C. for 20 hours. The reaction mixture was cooled to room temperature, diluted with toluene (1 L), and quenched with a small amount of water in a nitrogen atmosphere. The reaction mixture was filtered by using celite and washed three times with water by using a separatory funnel. The reaction mixture was dried by using anhydrous magnesium sulfate, filtered through a silica gel pad, and then, concentrated. The resultant obtained therefrom was recrystallized in a mixed solvent of ethanol_methanol=1:1 to obtain Intermediate 1-3. The amount of Intermediate 1-3 obtained was 156.1 g and the yield of Intermediate 1-3 was 55%.
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; Samsung Electronics Co., Ltd.; INAYAMA, Satoshi; IRISA, Shiro; KORAI, Keisuke; SAKURAI, Rie; ITO, Mitsunori; NUMATA, Masaki; (265 pag.)US2019/214570; (2019); A1;,
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