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ChemicalBook CAS DataBase List 1-(3-Chlorophenyl)-2-hydroxy-1-propanone

1-(3-Chlorophenyl)-2-hydroxy-1-propanone synthesis

8synthesis methods
34841-35-5 Synthesis
3'-Chloropropiophenone

34841-35-5
478 suppliers
$5.00/5g

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Yield: 96.2%

Reaction Conditions:

Stage #1:3'-chloro-propiophenone with 1-benzyl-3-methylimidazolium bis(trifluoromethanesulfonyl)imide salt in 2-methyltetrahydrofuran;N,N-dimethyl-formamide at 55; for 0.283333 h;
Stage #2: with 2,3-dicyano-5,6-dichloro-p-benzoquinone in 2-methyltetrahydrofuran;N,N-dimethyl-formamide at 55; for 3 h;Reagent/catalyst;Solvent;

Steps:

4 Example 5
At room temperature, to the proper amount of organic solvent (the volume ratio of 1:2 of the DMF 2-MeTHF mixture) in, adding 100mmol compounds represented by the following general formula (I) compound, 12mmol catalyst (to 5mmol asian tellurium with 7mmol mixture of iodizate bismith ) and 28mmol adjuvant 1-benzyl-3-methyl imidazolium- imide salt (trifluoro methane sulfonyl), and stirring and mixing 17 minutes, then heating to 55 °C, then adding 150mmol oxydizers DDQ, and the stirring reaction temperature is 3 hours
After the reaction, the reaction liquid is naturally cooled to the room temperature, add deionized water to dilute and full washing, then filtering, the filtrate by adding acetone extraction in 2-3 time, combined with the phase, drying anhydrous sodium sulfate, concentrated under reduced pressure, the residue 300-400 purpose silica gel column chromatography, to volume ratio of 1:2 and chlorofrom of a mixed solution of ethyl acetate to elute, so as to obtain the compound of formula (II), the yield is 96.2%.

References:

Zhang, Wei CN105348059, 2016, A Location in patent:Paragraph 0044; 0045; 0046, 0047; 0048

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