2,4-Dichlorophenylacetone synthesis

Yield:-

Reaction Conditions:

in tetrahydrofuran;toluene at -78 - 0; for 0.5 h;

Steps:

19.B

Step B. 1-(2,4-Dichlorophenyl)acetone. To a solution of 22.6 g (91.3 mmol) of the intermediate prepared in step A in 100 mL of THF at -78° C. was added 100 mL (140 mmol) of a 1.4 M solution of methylmagnesium bromide in THF/toluene. The reaction was warmed to ambient temperature and stirred for 30 minutes, then cooled to 0° C. and quenched by the addition of saturated aqueous NH4Cl. The mixture was diluted with 200 mL of EtOAc, and the organic layer washed with saturated aqueous NaHCO3, and brine, dried (MgSO4), and concentrated in vacuo. Purification by flash chromatography (10% EtOAc in hexane) afforded the title compound as a white solid. Mass spectrum (ES) m/e=203.0 (M+1).

References:

US2004/97552,2004,A1 Location in patent:Page 20