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ChemicalBook CAS DataBase List 2',4'-DIMETHYL-3-PHENYLPROPIOPHENONE
898764-27-7

2',4'-DIMETHYL-3-PHENYLPROPIOPHENONE synthesis

3synthesis methods
16017-30-4 Synthesis
1-ETHYNYL-2,4-DIMETHYL-BENZENE

16017-30-4
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Yield:898764-27-7 91%

Reaction Conditions:

Stage #1: 1-ethynyl-2,4-dimethylbenzenewith chloro(1,3-bis(2,6-di-i-propylphenyl)imidazol-2-ylidene)gold(I);water;silver trifluoromethanesulfonate in 1,4-dioxane at 120; for 1 h;Microwave irradiation;
Stage #2: benzyl alcoholwith bis[dichloro(pentamethylcyclopentadienyl)iridium(III)];potassium tert-butylate in 1,4-dioxane at 130; for 2 h;Microwave irradiation;

Steps:

19 1-(2,4-dimethylphenyl)-3-phenylpropan-1-one

The [(IPr) AuCl] (6mg, 0.01mmol, 1mol%), AgOTf (2.6mg, 0.01mmol, 1mol%), 2,4- dimethylbenzene acetylene (130mg, 1mmol), 1,4- dioxo six rings (1ml) and water (36ul, 2equiv.) were successively added to 5ml microwave tube.After the reaction mixture was microwaved at 120 reactor for one hour, cooled to room temperature.Thereto was added [Cp * IrCl2]2(8mg, 0.01mmol, 1mol%), potassium tert-butoxide (34mg, 0.3mmol, 0.3equiv.), Benzyl alcohol (130mg, 1.2mmol).After the reaction mixture was microwaved at 130 reactor and then reacted for 2 hours, cooled to room temperature.Filtered, and solvent was removed by rotary evaporation, then purified by column chromatography (developing solvent: petroleum ether / ethyl acetate) to give the pure title compound Yield: 91%

References:

CN104557500,2016,B Location in patent:Paragraph 0119; 0120; 0121; 0122

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