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3-(4-BROMOPHENYL)-4'-METHYLPROPIOPHENONE synthesis

5synthesis methods
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Yield:898760-99-1 90%

Reaction Conditions:

with C50H41ClIrNP2;caesium carbonate in benzene at 90; for 30 h;Schlenk technique;Inert atmosphere;

Steps:

14 example 14 Synthesis of 1-p-methylphenyl-3-p-bromophenyl-1-propanone:

To 10 ml of a Schlek reaction tube, 0.15 mmol of benzoquinoline triphenylphosphine ring iridium Hydrogen adduct (6), lmmol p-bromophenylacetylene, 2.2 mmol P-methylbenzyl alcohol, 1.5 mmol of cesium carbonate and 3 ml of benzene were charged and the reaction tube was replaced with nitrogen three times and then heated to 90 ° C with an oil bath under magnetic stirring and the reaction was refluxed for 30 hours. The filtrate was concentrated using a rotary evaporator and the remaining residue was purified by chromatography on oil (100 mL). The residue was purified by flash chromatography on silica gel eluting with an oil bath and the bath was cooled to room temperature. Ether as developing solvent, using silica gel thin layer chromatography to obtain pure product 1-p-methyl-phenyl-3-p-bromophenyl-1-acetone, the yield of 90%.

References:

CN103242372,2016,B Location in patent:Paragraph 0049; 0050

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