4'',5''-DICHLORO-2''-HYDROXYACETOPHENONE synthesis

Yield:22526-30-3 100%

Reaction Conditions:

Stage #1: 3,4-dichlorophenol;acetyl chloride at 60; for 2 h;
Stage #2: with aluminum (III) chloride at 60 - 180; for 0.5 h;

Steps:

298.1 Step 1.
1-(4,5-Dichloro-2-hydroxyphenyl)ethanone

Step 1.
1-(4,5-Dichloro-2-hydroxyphenyl)ethanone
A solution of 3,4-dichlorophenol [AK Scientific] (30 g, 18 mmol) in acetyl chloride (19 mL, 270 mmol) was stirred at 60° C. for 2 h.
The reaction mixture was cooled to 20° C., treated with aluminum trichloride (37 g, 280 mmol) portionwise, and heated at 180° C. for 30 min.
The reaction mixture was cooled to 20° C. and the solution hardened into a solid block that was not easy to break apart.
This material was cooled to 0° C. and quenched slowly with 1M HCl in portions.
The solid block of material slowly broke apart with enough HCl and this heterogenous mixture was stirred at 20° C. overnight to ensure uniformity.
The solid was filtered, washed with copious amounts of water, and dried under vacuum to give the desired product (38 g, quantitative) as a tan solid.

References:

US2014/249132,2014,A1 Location in patent:Paragraph 0486