Organic 2 Review Problem 227

Organic 2 Review Problem 227 - PREPARATIONS 211 thick...

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PREPARATIONS 211 thick viscous mass, which, however, will crystallise later and may then be easily broken up with the stirrer. When the addition of the diazo solution is complete, allow the mixture to stand in an ice-salt mixture for 30 minutes, with occasional stirring, and then filter the solution through a Buchner funnel under gentle suction from the pump: if the above directions have been carefully followed, filtration should be rapid. Wash the benzeneazo-2- naphthol well with water, and then drain thoroughly, pressing the crystals well down on to the filter with a spatula. Recrystallise one-third of the product from glacial acetic acid, reserving the remainder for reduction to i-amino-2-naphthol. (The azo- compound when dry is freely soluble, in acetic acid, but when moist is only moderately soluble: about 40 ml. of acetic acid are required for the portion recrystallised as above.) Filter the re- crystallised material at the pump, wash with a few ml. of ethanol or methylated spirit to eliminate acetic acid, and dry: yield, 3 g. Benzeneazo-2-naphthol is obtained as deep red crystals, m.p.
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This note was uploaded on 09/19/2011 for the course CHM 2211 taught by Professor Castalleano during the Fall '06 term at University of Florida.

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