Preparation of Pyrrolidine Pyrrolidine: 18 g of twice distilled from sodium pyrrole are dissolved in 60 ml of glacial acetic acid and hydrogenated with 0.5 g of platinum oxide. Absorption of hydrogen is throughout very slow and occasionally ceased completely, but the catalyst could be reactivated by shaking the reaction mixture with oxygen. Fresh portion platinum oxide (0.3 g) is added after 45 hours, and after 96-100 hours the theoretical amount of hydrogen has been absorbed. After the platinum has settled, the dark solution was decanted, the acetic acid was neutralized with concentrated solution of sodium hydroxide under a reflux condenser…
Author: Ethan Frank
Preparation of Aluminium Bromide Aluminium Bromide: The ideal vessel for this experiment is a 250 ml tabulated retort with a wide neck (at least 15 mm in diameter). However, a distilling flask of similar size with a delivery tube 15 cm long and 15 mm in diameter sealed on its neck may be used as a substitute. Aluminium Bromide: Sixty grams of bromine, previously dried with concentrated sulfuric acid are placed in a small dropping funnel with a long delivery tube. The neck of the funnel is protected with a drying tube. Ten grams of aluminum (30-mesh or turnings) are placed…
Preparation of 1-bromobutane 1-bromobutane: A mixture of 30 ml of water, 35 g of powdered sodium bromide and 25 ml (or 20 g) of 1-butanol are placed in a 250 ml round-bottomed flask. The flask is fitted with a dropping funnel with pressure-equalization arm. 25 ml of concentrated sulfuric acid is placed in the funnel and added dropwise into the reaction mixture with constant stirring and occasional cooling in an ice-water bath. When the addition of sulfuric acid is complete, the dropping funnel is replaced with a reflux condenser, and the reaction mixture is gently boiled for 45 minutes, shaking the…
Preparation of Acetaldehyde Ethanal Ethanal: To a 1-liter round bottom flask fitted with a dropping funnel, a distillation head with a condenser and mechanical stirrer 60 ml of concentrated sulfuric acid dissolved in 200 ml of water are placed. The diluted sulfuric acid is heated to boiling and 200 g of sodium dichromate in 200 ml of water which has been treated with 100 g of ethyl alcohol is then added in a small portion through the dropping funnel. During the addition of the sodium dichromate heat evolves and causes ebullition of the reaction mixture. The Ethanal, which forms during the…
Synthesis of Jones Reagent Jones Reagent: 7-[2-Methoxyimino-2-{2-(2,2,2-trifluoroacetamido)-1,3-thiazol-4-yl}acetamido]-3-hydroxymethyl-3-cephem-4-carboxylic acid (syn isomer) (1.0 g.) was dissolved in a mixture of dimethylformamide (6 ml.) and acetone (30 ml.). Jones reagent (1.25 ml.), which was prepared from conc. sulfuric acid (0.28 ml.), chromium trioxide (0.33 g.) and water (0.9 ml.), was dropwise added thereto over 2 minutes with stirring and cooling at 0° to 2° C. After stirring for 20 minutes at the same temperature, the reaction mixture was poured into ice-water (50 ml.). After acetone was distilled off, the residue was twice extracted with ethyl acetate (50 ml.). The extracts were washed with…
Synthesis of Magnesium Bicarbonate Magnesium Bicarbonate: The instant invention is based upon the discovery of a method for recovering extremely high purity magnesium carbonate from a magnesium hydroxide slurry. The magnesium hydroxide slurry can be produced in any conventional way, for example by adding lightly burned dolomite or lime, preferably the former, to sea water or the like to precipitate magnesium hydroxide, and then processing the precipitated hydroxide in a conventional way. The slurry can also be produced by suspending in water burned magnesite, burned dolomite or other natural or processed materials which will form magnesium hydroxide that can be…
Preparation of Acetyl Chloride Most commonly acetyl chloride prepared by the action of phosphorus trichloride on acetic acid, since acetyl chloride boils at 51° C and it is easily separated by simple distillation from the nonvolatile phosphorous acid. Phosphorus pentachloride reacts equally well, but in this case, the second reaction product is phosphorus oxychloride, which boils at 107° C and the separation is not easily accomplished. However, acetl chloride prepared from phosphorus oxychloride is very pure with very constant boiling and does not become turbid on standing. Preparation of acetl chloride with commonly used thionyl chloride is not practical as…
Preparation of Nitrobenzene Nitrobenzene: 81.5 ml of concentrated sulfuric acid (d=1.84 g/ml) are mixed gradually with frequent shaking with 71.5 ml of concentrated nitric acid (d=1.4 g/ml). After cooling the mixture to the room temperature, by immersion in a cold water bath, gradually, with constant stirring, 57 ml of benzene are dropwise added. If the temperature rises above 50-60° C, the nitration reaction is interrupted, and the flask is cooled with the ice water. When all of the benzene has been added, a reflux condenser is attached to the reaction flask and mixture is gently heated for an hour at…
Preparation of hydrogen iodide The HI 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. HI was distilled from the solid state and condensed in the receiver as white material.
Synthesis of Barium Phosphate Barium phosphate was prepared by the following procedure. Barium hydroxide (31.23 grams of Ba(OH)2 8H2O, 0.099 moles) was dissolved in 500 grams of deionized water and added to a 1 liter reaction flask fitted with a magnetic stirring bar, reflux condensor and dropping funnel. The hazy solution was heated to 68° C., and treated dropwise over a 30 minute period with a solution of 7.61 grams of 85%w phosphoric acid (0.066 moles of acid) in 50 grams of deionized water. The resulting milky white mixture was heated further at 80° C. for an additional two hours,…