Copper, vacuum filter productivity

Activated copper bronze is essential for satisfactory yields in the Ullmann reaction, and uniform results can be obtained by the following activation process. One hundred grams of copper bronze are treated with 1 litre of a 2 per cent solution of iodine in acetone for 5-10 minutes. This results in the production of a rather greyish colour due to the formation of copper iodide. The product is filtered off on a Buchner funnel, removed and washed by stirring with 500 ml of 1 1 solution of concentrated hydrochloric acid in acetone. The copper iodide dissolves, and the residual copper bronze is filtered and washed with acetone. It is then dried in a vacuum desiccator. The activated copper bronze should be used immediately after preparation. 

Summary CNTA is prepared by reacting 5-aminotetrazole with copper sulfate, and sodium nitrite in the presence of sulfuric acid. After the reaction, the mixture is cooled, and the product precipitates, forming a paste. The product is then vacuum filtered, washed, and dried. Commercial Industrial note For related, or similar information, see Serial No. 621,523, January 5th, 1937, by Edmund von Herz, Cologne, Germany. Part or parts of this laboratory process may be protected by international, and/or commercial/industrial processes. Before using this process to legally manufacture the mentioned explosive, with intent to sell, consult any protected commercial or industrial processes related to, similar to, or additional to, the process discussed in this procedure. This process may be used to legally prepare the mentioned explosive for laboratory, educational, or research purposes. 

Preparation of Copper(II) Bromide. Introduce 1-2 g of a copper powder into a beaker with 50 ml of water and while stirring the reaction mixture, slowly add 3-6 drops of bromine from a dropping funnel. When the reaction terminates, cool the solution, filter it through ordinary cotton wool inserted into a glass funnel, boil it with charcoal (for what purpose ), and evaporate it in a vacuum desiccator. Filter off the formed crystals on a funnel with a filtering bottom. What is the composition of the product Write the equation of the reaction. Test how the copper bromide crystals behave in water and when heated. To do this, put 5-6 small crystals of the salt into each of two test tubes. Carefully add water dropwise to one of the tubes until the solution acquires a light blue colour, and then introduce about 0.2 g of dry potassium bromide, and heat the second tube. What happens Explain the observed phenomena. 

Five grams of copper sulfate 5-hydrate are dissolved in 20ml of water and 3.5g of dipropylenetriamine are added with stirring. Acetone is added to the blue liquid until the product has been completely precipitated as an oil the supernatant liquid should be almost colorless. The oil is repeatedly triturated with small portions of acetone in a mortar until it forms a solid it is brought onto the filter with the same solvent and washed with a little ether. While the deep blue product is still moist, it is rapidly transferred to a vacuum desiccator and pumped dry. The material is extremely deliquescent. Losses in the preparation are only mechanical. The complex sulfate gives no precipitate with solutions of iodide, dithionate, ferricyanide, or persulfate ions. In concentrated aqueous medium, however, the addition of solid sodium fluoroborate causes partial precipitation of the relatively insoluble complex fluoroborate. 

The ligand H4daen (3.32 g, 0.01 mole) is dissolved in the minimum volume of hot dichloromethane and added to a solution of copper(II) acetate monohydrate (2.00 g, 0.01 mole) dissolved in the minimum volume of hot 95% ethanol. The resulting solution immediately becomes dark green, and after it is warmed on a steam bath a fine, shiny-brown microcrystalline solid precipitates. The mixture is allowed to cool and the product is collected by filtration. The complex is purified by suspending it in hot toluene and then filtering. This procedure is carried out three times. The pure complex is dried under vacuum. The yield is 2.3 g (60%). Anal. Calcd. for C18H26N402Cu C, 54.8 H, 6.6 N, 14.2. Found C, 54.6 H, 6.7 N, 14.3. 

Procedure Add 20 grams of picryl chloride and 400 milliliters of ethylene dichloride to a 1-liter flask equipped with a stirrer, thermometer, and condenser. Then stir the mixture to fully dissolve the picryl chloride. Afterwards, heat the mixture to 75 Celsius. When the temperature of the mixture reaches 75 Celsius, slowly add in small portions, 8.8 grams of copper powder while rapidly stirring the picryl chloride mixture. After the addition of tire copper powder, reflux the reaction mixture at 84 Celsius for two hours. After which, remove the heat source, and allow the mixture to cool to room temperature. Then filter-off the precipitated product, wash with 400 milliliters of water, and then vacuum dry or air-dry the product. Then recrystallize the product from 100 milliliters of acetone, and then wash with 400 milliliters of water. Then vacuum dry or air-dry the product. 

Into a metal pressure reactor were placed copper pentafluorobenzenethiolate (20 5.3 g, 20 mmol), tri-fiuoioiodoethene (21 5.0 g. 24 mmol), and DMAC (20 mL). The reactor was sealed and heated to and maintained at 70 C for 20 h. On cooling, an aliquot sample was removed, and added to EtjO which was repeatedly washed with HjO, and then analyzed by GC. Analysis indicated a trace of DMAC and only one major product peak, besides the solvent. The contents of the reactor were poured into a mixture of EtjO (50 mL) and H2O (100 mL). The mixture was filtered to remove the Cul and the EtjO layer was separated, dried (MgSO ), and subsequently concentrated under vacuum to yield the crude product (5.0 g). The crude product was distilled to give pure 22 yield 65%. 

The solution was cooled to room temperature and then filtered into a Buchner funnel with the aid of a water aspirator and the filtrate evaporated in a rotary evaporator. The yellow residue was taken up in dichloromethane (80 mL), filtered again and then the organic layers were washed with water (2 x 30 mL) and brine (1 x 30 mL) in a separatory funnel. The combined aqueous layers were back extracted with dichloromethane (30 mL). The combined organic layers were dried over anhydrous magnesium sulfate and evaporated to dryness to leave the desired compound as a yellow gel (2.96 g, 92%). The purity of the crude product is high enough to be used in the copper complex synthesis, but can be further purified by vacuum distillation of the unreacted salicylaldehyde. 

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