Distilling ethers to dryness
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In view of the small volume of nitromethane to be manipulated, the crude nitromethane may be extracted from the aqueous distillate with ether ml. Dry the ethereal extract over sodium sulphate , filter through a fluted filter-paper , and then distil off the ether on a water-bath with the usual precautions Fig. Then run off the lower aqueous layer , and shake the ethereal solution with about an equal volume of dilute sulphuric acid to remove traces of foul-smelling phenyl isocyanide CaHjNC which are always present.
Finally separate the sulphuric acid as completely as possible, and shake the ether with water to ensure absence of acid. Run off the water and dry the benzonitrile solution over granular calcium chloride for about 20 minutes. Replace the aqueous layer in the funnel, and extract similarly twice more with ether, combining the ethereal extracts in the conical flask. Add g. The ethereal solution of the phenol Then add 15 g.
Continue precisely as in the preparation of anisole, shaking the ethereal extract with sodium hydroxide solution as before in order to eliminate any unchanged phenol. Yield, 14 g. Run in 35 g 42 nil, of - hexyl methyl ketone , and continue the heating and vigorous stirring for ij hours. The mixture can conveniently be set aside overnight after this stage.
Extract the oily oxime from the cold mixture twice with ether. Wash the united ethereal extract once with a small quantity of water, and dry it with sodium sulphate. Then distil off the ether from the filtered extract , preferably using a distillation flask of type shown in Fig. Collect the liquid ketoxime, b. Yield, g. Pour the mixture into a separating-funnel , and rinse out the flask or basin with ether into the funnel.
Extract the mixture twice with ether 2 X25 ml. Dry the united ether extracts over flake or powdered sodium hydroxide, preferably overnight. Distil the dry filtered extract from an apparatus similar to that used for the oxime when the ether has been removed, distil the amine slowly under water-pump pressure, using a capillary tube having a soda-lime guard - tube to ensure that only dry air free from carbon dioxide passes through the liquid.
Collect the amine, b. Yield, 18 g. Rinse out the flask which may contain some unchanged zinc with ether, pour the latter into the funnel, and extract the aqueous solution with the ether. Repeat the extrac tion with a second quantity of ether, unite the ether extracts, wash them by extracting once with water , and then dry the ethereal extract over sodium sulphate. When the ether has been removed, replace the water-condenser by an air-condenser, and continue When the ether has been removed, fit a capillary tube and thermometer, and continue the distillation at water-pump pressure.
The diethyl ester of collidine-3,5- dicarboxylic acid II distils as a pale golden oil, b. Yield, 5 g. Transfer the mixture to a separating-funnel , wash out the beaker with ether, adding the washings also to the solution in the funnel, and then extract the quinoline twice with ether. Dry the united ethereal extracts by adding an ample quantity of powdered potassium hydroxide and Extract the distillate thoroughly with ether ca. Filter the dry extract through a fluted filter-paper moistened with ether into a ml.
Fit the flask with a distillation-head , or a knee-tube , and distil off the ether. Now replace the distillation-head by a reflux water-condenser , add 10 ml. Dissolve I ml. HCl and add sodium nitrite solution gradually with shaking until the yellow oil separates out at the bottom of the solution. Transfer completely to a smdl separating-funnel , add about 20 ml. Run off the lower layer and wash the ethereal extract first with water , then with dil.
A transparent lid is ideal, as it will allow you to see what is happening. You can also place some ice packs or cool water on top of the lid to help the vapor cool faster and return to a liquid form. Turn on the stove and heat the water. Monitor the temperature of the water and keep it at a slow boil.
You want to avoid heating the water too much and having the dirty water splashing into your collection pot. Adjust the temperature as needed. Do not boil the pot dry or you will risk causing permanent damage to it. Let the distilled liquid cool. It may take several hours of boiling to collect a significant amount of liquid, so be patient.
Generally, simple distillation as described here will work for substances that boil below oC. Above that, many compounds can decompose, so a vacuum distillation is recommended. If you don't know the boiling point of the substance you want to distill, a very rough rule of thumb is that a compound's boiling point rises by around 15 oC for each carbon that's added to the chain.
Find a compound structurally similar to the one you want to distill, and add 15 oC per additional carbon. Take the liquid you want to purify and pour it into the distilling flask. Only fill the flask between half and two-thirds full, so the liquid does not take too long to evaporate.
You can use a stand to hold the flask above the burner or heat source. You may also want to use a basin filled with sand to rest the distilling flask on instead of directly over the burner. This will prevent the liquid from boiling too violently as the sand helps to evenly distribute the heat.
Attach one end of the condenser to the vent at the top of the distilling flask. The condenser should be angled downward to help the water flow toward the collection flask. The condenser will transfer the vapor to the collection container and help to cool it back into a liquid form. This is a piece of glassware with a vacuum adapter, an inlet, and several outlets for connecting flasks. Make sure to grease the joint between the pig and the condenser, so you can change fractions easily.
Place the cup or flask beneath the opening on the end of the condenser. The liquid will drip out as the vapor cools and collect in the cup below. Bring the liquid to a boil and monitor the temperature. You may want to use a thermometer to monitor the temperature and keep the liquid just above the boiling point so it doesn't heat too quickly. Adjust the burner level if needed.
For a while the thermometer's temperature will not change, but once enough vapour builds up, the temperature should rise rapidly, and then level off. This value is the compound's boiling point at the pressure. Turn the heat off once the distilling flask is mostly empty. Do not heat the flask until dry as you could damage the glass.
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