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ChemicalBook CAS DataBase List 2-Amino-5-bromobenzotrifluoride

2-Amino-5-bromobenzotrifluoride synthesis

10synthesis methods
-

Yield:445-02-3 92%

Reaction Conditions:

with potassium carbonate in acetonitrile at 75; for 6 h;Schlenk technique;Inert atmosphere;

Steps:

3. General procedure for the reaction
General procedure: Experimental Procedure: A dried 25 mL Schlenk tube equipped with a magnetic stir bar was charged with Togni’s Reagent 2 (0.25 mmol, 1.0 equiv), free anilines 1 (0.75 mmol, 3.0 equiv), K2CO3 (0.375 mmol, 1.5 equiv) and CH3CN (1.5 mL). The reaction mixture was then stirred at 75 °C for 6 h under an argon atmosphere. The reaction progress was monitored by TLC. After cooling to room temperature, the mixture was washed with water and extracted with CH2Cl2 three times, then washed with saturated NaCl solution. The combined organic layer was dried with anhydrous Na2SO4 and filtered. The filtrate was concentrated in vacuo. The crude product was purified by flash column chromatography on silica gel (Elutent: petroleum ether-EtOAc) to give the pure product. The products were characterized by 1H NMR, 13C NMR, 19F NMR, GC -MS.

References:

Chen, Xiaoyu;Ding, Licheng;Li, Linlin;Li, Jingya;Zou, Dapeng;Wu, Yangjie;Wu, Yusheng [Tetrahedron Letters,2020,vol. 61,# 9,art. no. 151538] Location in patent:supporting information

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