Preparation of p-benzoquinone (benzoquinone; quinone) Benzoquinone: Quinone usually is prepared by the oxidation of aniline in acid solution with sodium dichromate. On a laboratory scale the yield is only about 35% and the process is somewhat lengthy. A rapid method of preparing pure quinone consists in oxidizing hydroquinone with manganese dioxide in an acid medium and removing the product from the reaction mixture by steam distillation. Oxidation of hydroquinone is a more satisfactory regarding starting material than aniline for the laboratory production of quinone. Furthermore, the yield is much better. The reaction is carried out in a 2-liter flask having a…
Author: Ethan Frank
Preparation of Potassium Nitrite Potassium nitrite is prepared (similarly to sodium nitrite) by heating potassium nitrate with elemental lead. Lead also could be replaced with metallic copper or zinc. In an iron pan a mixture 100 g of potassium nitrate and 204 g of metallic lead is fused with proper stirring. Even at a low red heat the lead becomes for the most part oxidized and converted into a yellow powder – lead oxide (PbO). To finish the reaction and oxidize completely remaining lead, the heat is increased to visible redness and maintained with stirring at that point for 30 minutes.…
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Preparation of Lead II Nitrate Lead II Nitrate: Lead nitrate is one of the most readily prepared salts of lead. Lead oxide (litharge), lead carbonate or metallic lead is treated with an excess amount of concentrated nitric acid. When the reaction mixture cools the crystals of lead(II) nitrate crystallizes. Lead(II) nitrate is separated by filtration and purified by recrystallization. If an insufficient amount of nitric acid is used, the basic salt of lead nitrate (Pb(OH)NO3) forms, which separates as a fine granular or flaky precipitate when the solution cooled. Lead II Nitrate: Synthetic inorganic chemistry, by A. A. Blanchard, 277-278, 1936…
Preparation of Nitrogen Trichloride Nitrogen Trichloride: In 1 liter round bottom flask 225 ml of chloroform with 10-20% carbon tetrachloride is placed. To this mixture 600 ml of a 10% solution of ammonium sulfate was added. The flask is plugged with stopper having inlet and outlet tubes. The outlet tube is attached to a flask containing an excess of alkali to absorb chlorine. To control the reaction the flask should be cooled with ice-water. Then, the inlet tube is attached to the chlorine generator and strong current of chlorine while shaking the reaction mixture is passed into the solution for…
Preparation of Ammonium Hydroxide Ammonium hydroxide is prepared by saturating water with gaseous ammonia. Ammonia gas is generated and conducted directly from the flask without the introduction of a drying tube into an empty gas washing-bottle which serves to collect any solid particles mechanically carried over. Gaseous ammonia is prepared by gently heating crude ammonium chloride (or ammonium sulfate) with dry calcium hydroxide: Powdered ammonium chloride and calcium hydroxide in equal quantities are placed in Erlenmeyer flask fitted with a glass elbow. On the application of gentle heat ammonia is rapidly evolved. The gas is then conducted through a series of…
Preparation of Benzoyl Chloride Benzoyl chloride could be prepared by reacting thionyl chloride or phosphorus pentachloride with benzoic acid. 50 grams of dry benzoic acid are treated in a 500 ml flask, with 90 grams of finely pulverized phosphorus pentachloride. The mixture is mixed well, upon which, after a short time, the reaction takes place with an energetic evolution of hydrochloric acid, and the reaction mass becomes liquid. During the reaction a lot of heat is released. After standing a short time, the completely liquid mixture is twice fractionated by collecting fraction which boils at ~ 200° C, yielding 90 %…
Preparation of Hydrogen Iodide The hydrogen iodide could be obtained by dehydrating hydroiodic acid with phosphorus pentoxide. The concentrated solution of hydroiodic acid added dropwise to the phosphorus pentoxide. The gas evolved was purified by passing trough a tube filled with phosphorus pentoxide and condensed with liquid nitrogen. Hydrogen iodide was distilled from the solid state and condensed in the receiver as white material.
Preparation of Iron iii Nitrate Iron iii Nitrate: To a mixture of 100 ml of concentrated nitric acid and 30 ml of water, 50 g of iron filings or fine turnings in small portions are added. The rate of reaction can be regulated by the rate of addition of iron and by gently heating the mixture but not above 70° C. When the iron has practically all dissolved, the solution is filtered and set it aside to crystallize. The filtrate is usually dark in color owing to the presence of colloidal basic nitrates. These salts are gradually converted into the…
Preparation of Cinnamic Acid Cinnamic Acid: A mixture of 20 grams of benzaldehyde, 30 grams of acetic anhydride, both freshly distilled, and 10 grams of anhydrous pulverized sodium acetate, is heated in a flask fitted with a reflux condenser, for 8 hours, at 180° C. After the reaction is complete, the hot reaction product is poured into a large flask. Water is added and then distilled with steam, until no more benzaldehyde passes over. The quantity of water used here is large enough so that all of the cinnamic asid dissolves except a small portion of an oily impurity. The…