[makfc]

I'm preparing 3-acetoxy-Phenacylbromide from 3-acetoxyacetophenone. For this, I found abstract of one article of FARMACO, 48; 6; 1993; 857-869, in which Dioxane, ether & Br2 was used giving 100% yield of the brominated compound.

Unfortunately, I could not find fulltext of this article from our university library or anywhere else. 

Can anyone pls suggest me the experimental details of this process or this article ?

Pls help...

[GSR]

hi,
here is some procedure


A solution of 50 g. (0.42 mole) of acetophenone in 50 cc. of pure anhydrous ether is placed in a dry three-necked flask fitted with a separatory funnel, mechanical stirrer, and reflux condenser . The solution is cooled in an ice bath, 0.5 g. of anhydrous aluminum chloride is introduced, and 67 g. (21.5 cc., 0.42 mole) of bromine is added gradually from the separatory funnel, with stirring, at the rate of about 1 cc. per minute. The bromine color disappears rapidly although very little hydrogen bromide is evolved; towards the end of the reaction the solution becomes pink.
After the bromine has been added the ether and dissolved hydrogen bromide are removed at once  4) under reduced pressure with a slight current of air. The phenacyl bromide remains as a solid mass of brownish yellow crystals ; the color is removed by shaking with a mixture of 10 cc. of water and 10 cc. of petroleum ether. The crystals are filtered with suction and washed several times with fresh portions of the solvent mixture, if necessary, until a white product is obtained . The crude phenacyl bromide weighs 74–80 g. (88–96 per cent of the theoretical amount) and melts at 45–48°. . If higher purity is desired the crude product may be recrystallized from 25–30 cc. of methanol, yielding 54–55 g. (64–66 per cent of the theoretical amount) of white crystals melting at 49–51° .


cheers
GSR

[makfc]

Ya..

But I'm still looking for the requested procedure which does not use AlCl3..

[GSR]

well...
 in that case you may have to purchase that article.

GSR