PROSEDUR ASLI (Wertheim E)

In a 500 cc Florence flask place 10 g of iodine and pour on to this 10 g of acetone. Add small portions, and with constant shaking, as much as is needed of a solution made up of 20 cc of 8 N sodium hydroxide solution and 80 cc of water. If the flask becomes hot to the hand, cool it at once with running water. When sufficient sodium hydroxide solution has been added set the flask aside. No free iodine should be present at this time, nor any suggestion of brown color in the liquid. Look carefully on the bottom of the flask for unattacked iodine. After 5 minutes collect the yellow precipitate, using the small Buchner funnel. Place filtrate at once in bottle labeled Iodoform filtrate. Wash the solid on the funnel with a little water. The compound is then to be dissolved in the smallest possible quantity of hot ethyl alcohol as follows: put the iodoform in a small flask arranged for refluxing. Pour a few cc of alcohol down the condenser (no flames with 6 L), and warm on the electric hot plate or the steam-bath, shaking the flask at times. When the mix is warm add a little more alcohol, then wait till it becomes hot to see whether enough has been added to dissolve all (there will always be a few shreds of filter paper, etc, which should not be mistaken for iodoform). Do not heat longer than necessary and avoid actual boiling if possible. When enough solvent (about 40 cc) has been added to dissolved all the iodoform at the boiling point of the solution, add about 2 cc additional solvent, then filter the hot solution through a fluted filter paper, using a funnel previously warmed over the hot plate or steam-bath. Caution: Do not inhale the vapor from the solution. Cover the filtered solution and set aside to cool slowly. In 15 minutes add about 25 cc of water, meanwhile stirring vigorously to completely precipitate the iodoform, and then filter with the Buchner. Wash the crystal on the funnel with a few drops of cold alcohol (cut off suction during the washing). Remove the crystal from the filter paper and spread them on a fresh, dry piece of filter paper. The best

way to remove paper, etc, from the Buchner funnel is to hold it over a clean filter paper and blow gently through the steam. The end of the funnel-stem should first be washed so that no chemicals can get on the lips. Any crystals remaining in the funnel are removed with knife or spatula. The crystals are to be placed in the desiccators. Place an identification slip in the desiccators. Products in course of preparation should always be labeled; do not rely on the memory. The bottom of the desiccators should contain granules of calcium chloride to a depth of about 15 mm. the melting point and weight of the preparation will be determined after it is dry, at the next laboratory period. For directions for melting point determinations see expt 4, submit the product in a sample bottle, properly labeled.