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866821-66-1

3'-BROMO-3-PHENYLPROPIOPHENONE synthesis

10synthesis methods
-

Yield:866821-66-1 75%

Reaction Conditions:

with 2,4,6-trimethyl-pyridine;[7-(dimethylamino)phenothiazin-3-ylidene]dimethylazanium chloride;triphenylphosphine in N,N-dimethyl acetamide at 20;Inert atmosphere;Irradiation;

Steps:

12

Weigh (28mg, 0.2mmol), photocatalyst Methylene blue (5.6mg, 2%), 2,4,6-trimethylpyridine (24mg, 0.2mmol) and triphenylphosphine (78.6mg, 0.3mmol) were added to the reaction flask, replaced with nitrogen three times, styrene (31mg, 0.3mmol) was dissolved in 2mL of N,N-dimethylacetamide solvent, under nitrogen atmosphere, slowly add to the reaction flask, place the reaction flask under white LEDs, and react at room temperature for 24-36h. After the reaction is over, add 15 mL of water, extract with ethyl acetate (3x10 mL), stand still, separate into layers, pour out the lower aqueous phase, combine the organic phases, dry the organic phase with anhydrous sodium sulfate, and evaporate the organic phase, dry loading, column chromatography (petroleum ether: ethyl acetate) to obtain 43 mg of the target product with a yield of 75%.

References:

CN111978168,2020,A Location in patent:Paragraph 0037-0038

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