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DIBROMOACETOPHENONE synthesis

13synthesis methods
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Yield: 89%

Reaction Conditions:

with 1,3-dibromo-5,5-dimethylimidazolidine-2,4-dione in 1,2-dimethoxyethane;water at 80; for 4 h;

Steps:

Control experiments
DBH (143 mg, 0.5 mmol) and 2-bromo-1-phenylethanol (3) (50 mg, 0.25 mmol) were added into DME-water (1.35 mL : 0.3 mL) at rt. The resultant mixture was heated to 80 °C and stirred for 4 h. Then the mixture was quenched by saturated sodium bicarbonate (1 mL), extracted with ethyl acetate, washed by brine, and dried over Na2SO4 subsequently. After concentrated in vacuo, the crude product was purified by prepared thin layer chromatography to give dibromoketone 2a (62 mg, 89%).

References:

Wu, Ping;Xu, Senhan;Xu, Hao;Hu, Haiyan;Zhang, Wei [Tetrahedron Letters,2017,vol. 58,# 7,p. 618 - 621] Location in patent:supporting information

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