Norit

On the whole it is better to employ the activated decolourising charcoal prepared from wood. Excellent decolourising carbons are marketed under the trade names Norit (from birch wood), Darco and Nuchar. ... 

Purification of charcoal. Heat Norit charcoal on a water bath for 6 hours with 10 per cent, nitric acid, filter, wash free from acid, and dry at 100°. If the acid-washed form of Norit charcoal is available, it may be used directly without further purification. 

Any of the commercial forms of activated carbon (Norit, Darco, etc.) may be employed the carbon should be heated on a steam bath with 10 per cent, nitric acid for 2-3 hours, washed free from acid with water, and dried at 100-110° before use. 

Indoleacetic acid In a 1-litre flask, fitted with a reflux condenser, place a solution of 35 2 g. of sodium cyanide in 70 ml. of water, then add 25 g. of gramine and 280 ml. of 95 per cent, ethanol. Reflux the mixture (steam bath) for 80 hours. Dilute the cooled reaction mixture with 35 ml. of water, shake with a little activated charcoal (e.g., Norit), filter and concentrate to about 350 ml. imder reduced pressure (water pump) in order to remove most of the alcohol. Cool to about 5°, filter off the solid and wash it with a little cold water keep the filtrate (A). Recrystallise the solid from alcohol-ether to give 5-0 g. of 3-indoleacetamide, m.p. 150-151°. 

Property Manufacturer Calgon Coal Norit Peat Westvaco Calgon Norit Peat Westvaco Wood... 

The estimated production capacity of activated carbon in the United States is shown in Table 3 for seven manufacturers (41). The principal producers are Calgon Carbon (37%), American-Norit (26%), Westvaco (19%), and Atochem (10%). Several other companies purchase activated carbon for resale but do not manufacture products. 

Western Europe has seven manufacturers of activated carbon. The two largest, Norit and Chemviron (a subsidiary of Calgon), account for 70% of West European production capacity, and Ceca accounts for 13% (42). Japan is the third largest producer of activated carbon, having 18 manufacturers, but four companies share over 50% of the total Japanese capacity (43). Six Pacific Rim countries account for the balance of the world production capacity of activated carbon, 90% of which is in the Philippines and Sri Lanka (42). As is the case with other businesses, regional markets for activated carbon products have become international, lea ding to consoHdation of manufacturers. Calgon, Norit, Ceca, and Sutcliffe-Speakman are examples of multinational companies. 

Product data bulletins from activated carbon manufacturers, Calgon Carbon Corp., 1990, American Norit Co., 1990, and Westvaco Corp., 1988. 

If the material is not partly dried before hydrolysis, the yield of the hydrochloride is diminished because of its solubility. If pure 3-bromo-4-acetaminotoluene is desired, the crude material may be crystallized from 50 per cent alcohol with the addition of decolorizing carbon (Norite) as almost colorless needles, m.p. 116-117°, The yield is 360 g, (79 per cent of the theoretical amount). This purification has no advantage when the acetam-ino compound is to be hydrolyzed to the amine. 

In a 500-cc. round-bottom flask fitted with a reflux condenser are placed 68 g. of phenylurea (0.5 mole) (Note i) and 120 cc. (i mole) of 42 per cent hydrazine hydrate solution (Note 2). The flask is heated on a steam bath for about twelve hours. The hot mixture is treated with a small amount of decolorizing charcoal (Norite) and filtered. The charcoal is washed with two 15-CC. portions of warm water and the filtrate and washings are then concentrated on a steam bath to about 100 cc. On coolipg in an ice bath a crop of crystals separates and is collected on a filter and washed with two 15-cc. portions of cold water. The filtrate and washings are concentrated to about 25 cc. and another crop of crystals is obtained as before. The total yield of crude compound is 47-52 g. It is white at first but sometimes turns brown on drying. It usually melts below 115° because of some unchanged phenylurea. 

For the hydrolysis, 36 g. (O.ll mole) of the residue is transferred to a 1-1. round-bottomed flask equipped with a reflux condenser, and 210 ml. of concentrated hydrochloric acid in 190 ml. of water is added. The mixture is refluxed gently at first, then vigorously (Note 6), until hydrolysis is essentially complete (about 20 hours). Then 180 ml. of W ater and 4 g. of Norite A are added and the mixture is stirred and boiled for 3 minutes, after which it is rapidly filtered with suction through two layers of hardened filter paper in a Buchner funnel (Note 7). The filtrate, upon cooling to 20° or below, deposits 18 g. (72%) of lightly colored 2,5-dihydroxy- -benzenediacetic acid (Note 8). A snow-... 

C. Saponification. The ester is saponified by refluxing for 5 hours with 75 ml. of a 10% sodium hydroxide solution containing 3 ml. of ethyl alcohol it is then poured into 150 ml. of water and decolorized with Norite. Upon acidification of the alkaline solution with dilute hydrochloric acid, 18-19 g. (40-43%) (Notes 7 and 8) of acid is obtained, melting at 191-193° (corr.). 

To 40 g. of dry chitin in a 500-ml. beaker is added 200 ml. of concentrated hydrochloric acid (c.p., sp. gr. 1.18), and the mixture is heated on a boiling water bath for 2.5 hours with continuous mechanical agitation. At the end of this time solution is complete, and 200 ml. of water and 4 g. of Norite are added. The beaker is transferred to a hot plate, and the solution is maintained at a temperature of about 60° and is stirred continuously during the process of decolorization. After an hour the solution is filtered through a layer of a filter aid such as Filter-Cel. The filtrate is usually a pale straw color however, if an excessive color persists, the decolorization may be repeated until the solution becomes almost colorless. The filtrate is concentrated under diminished pressure at 50° until the volume of the solution is 10-15 ml. The white crystals of glucosamine hydrochloride are... 

The product is pure enough for most uses. If a purer product is desired, the crystals may be dissolved in the minimum amount of boiling water and treated with Norite. The resulting solution is filtered and added to a large excess of 95% alcohol and stirred vigorously for several hours. The product is collected after 4 to 6 hours. An appreciable amount of the d-form of the amino sugar remains dissolved in the alcohol and may be precipitated by adding ether. 

The catalyst is previously prepared in an apparatus for catalytic hydrogenation, in which are placed 0.5 g. of palladous chloride, 3.0 g. of Norite, and 20 ml. of distilled water. The bottle is swept out with hydrogen and then shaken with hydrogen for 2-3 hours at 2-3 atmospheres (40 lb.) pressure. The palladium on carbon is collected on a Biichner funnel, washed with five 50-ml. portions of distilled water, then with five 50-ml. portions of 95% ethanol, and finally twice with ether. Upon drying, about 3 g. of the catalyst is obtained. It is stored in a vacuum desiccator over solid sodium hydroxide. If the reduction of the chloro-lepidine does not proceed normally, the used catalyst should be removed by suction filtration and a fresh 3-g. portion of catalyst added. Failure of the reduction step is usually due to an inactive catalyst or to impurities in the acetic acid or chlorolepidine. The palladium catalysts, prepared as described elsewhere in this volume, are presumably also satisfactory for the reduction of 2-chlorolepidine (p. 77). 

Norite, is heated to boiling by introduction of steam, filtered through a Norite filter pad by suction, and cooled in an ice-salt bath. The muconic acid is precipitated by the addition of a large excess (1500 ml.) (sp. gr. 1.18) of concentrated hydrochloric acid to the cold solution. The acid is added in a thin stream to the well-stirred solution. After 2 hours the muconic acid is filtered, washed first with two 400-ml. portions of cold water and then with 200 ml. of methyl alcohol, and dried at 85°. The yield of nearly colorless product melting at 296-298°, with decomposition, amounts to 165-195 g. (37-43%). 

Norite, Darco, or other carbons may be used. The carbon is heated on a steam bath with 10% nitric acid for 2 to... 

In a 250-ml. flask attached to a Vigreux column 30 cm. in over-all length ("Note 1) a mixture of 42.8 g. (0.2 mole) of phenyl salicylate ( Salol, m.p. 42-43°), 26.7 g. (0.25 mole) of o-tolui-dine, and 60 g. of 1,2,4-trichlorobenzene (m.p. 15-16°), is heated at the boiling point, so that the phenol formed slowly distils. The temperature rises from 183° to 187° during the first hour, and 22-23 g. of distillate is collected. Heating is continued until the temperature rises to 202° and a total of 45-46 g. of distillate has been collected (Note 2). The flask is then removed, and to it are added 3 g. of Norite and 10 nil. of trichlorobenzene. The mixture is heated to boiling and filtered hot by suction. The... 

The checkers preferred o -methylnaphthalene (Eastman, Practical) as the diluent. When it is used in the apparatus described the phenol does not distil, so that a reaction flask fitted with an air-cooled condenser is more convenient. The reactants in 60 g. of -methylnaphthalene are heated in an oil bath at 230° for 1.5 to 2 hours. Three grains of Norite and 20 g. more of a-methylnaphthalene are then added, and the mixture is treated as described in the Procedure. The yield and melting point of the product are identical with those described. 

Charcoal is generally satisfactorily activated by heating gently to red heat in a crucible or quartz beaker in a muffle furnace, finally allowing to cool under an inert atmosphere in a desiccator. Good commercial activated charcoal is made from wood, e.g. Norit (from Birch wood), Darco and Nuchar. If the cost is important then the cheaper animal charcoal (bone charcoal) can be used. However, this charcoal contains calcium phosphate and other calcium salts and cannot be used with acidic materials. In this case the charcoal is boiled with dilute hydrochloric acid (1 1 by volume) for 2-3h, diluted with distilled water and filtered through a fine grade paper on a Buchner flask, washed with distilled water until the filtrate is almost neutral, and dried first in air then in a vacuum, and activated as above. To improve the porosity, charcoal columns are usually prepared in admixture with diatomaceous earth. 

Diacetyl benzene [1009-61-6] M 162.2, m 113-5-114.2 . Crystd from benzene and vacuum dried over CaCl2. Also dissolved in acetone, treated with Norit, evapd and recrystd from MeOH [Wagner et al. J Am Chem Soc 108 7727 1986]. 

Glutaraldehyde [111-30-8] M 100.1, b 71 /10mm, as 50% aq soln. Likely impurities are oxidation products - acids, semialdehydes and polymers. It can be purified by repeated washing with activated charcoal (Norit) followed by vacuum filtration, using 15-20g charcoal/KKhnL of glutaraldehyde soln. 

Luminol (5-aminophthalazin-l,4-dione) [521-31-3] M 177.2, m 329-332°, pK] 3.37, pK2 6.35. Dissolved in KOH soln, treated with Norit (charcoal), filtered and ppted with cone HCl. [Hardy, Sietz and Hercules Talanta 24 297 1977.] Stored in the dark in an inert atmosphere, because its structure changes during its luminescence. It has been recrystd from O.IM KOH [Merenyi et al. J Am Chem Soc 108 77716 1986]. 

Trioxsalen (2,5,9-trimethyl-7H-furo[3,2-g]benzopyran-7-one) [3902-71-4] M 228.3, m 233-235 , 234.5-235 . Purified by recrystn from CHCI3. If too impure it is fractionally crystd from CHCl3-pet ether (b 30-60°) using Norit and finally crystd from CHCI3 alone to give colourless prisms, m 234.5-235°. It is a photosensitiser so it should be stored in the dark. [UV Kaufmann J Org Chem 26 117 1961-, Baeme et al. J Chem Soc 2976 1949.]... 

Cupferon ammonium salt (7V-nitroso-7V-phenylhydroxylamine ammonium salt) [135-20-6] M 155.2, m 150-155°(dec), 162.5-163.5°, 163-164°, pK 4.16 (free base). Recrystd twice from EtOH after treatment with Norite and finally once with EtOH. The crystals are washed with diethyl ether and air dried then stored in the dark over solid ammonium carbonate. A standard soln (ca 0.05M prepared in air-free H2O) is prepared daily from this material for analytical work and is essentially 100% pure. [Anal Chem 26 1747 1954.] It can also be washed with Et20, dried and stored as stated. In a sealed, dark container it can be stored for at least 12 months without deterioration. Xmax 260nm (CHCI3). [Org Synth Coll Vol I 77 1948 J Am Chem Soc 78 4206 7956.] Possible CARCINOGEN. 

The hot solution is very destructive to filter paper. A convenient filter is made by preparing a 1-2 mm. mat of asbestos in a 6-cm. Buchner funnel, dusting onto this a 2-5 mm. layer of Norite, washing by suction, and heating the unit, together with a suction flask, in an oven at 120°. When dry and hot, the apparatus is ready for use. 

The benzene solution is separated and washed twice with 100 cc. of water, once with 200 cc. of 5 per cent potassium hydroxide, and twice with water, and in case the solution is not colorless it is clarified with i g. of Norite. The benzene is removed by distillation and the resulting syrup is dissolved in 300 cc. of alcohol by heating. The solution on cooling deposits cholestanone as well-formed needles. The yield of collected, washed, and air-dried material, m.p. 129-130°, is 41.5-42 g. (83-84 per cent of the theoretical amount). The addition of 80 cc. of water to the filtrate gives about 2 g. of material melting at 125-126°. 

If very pure amine is desired the product described above is dissolved with 1.04 parts of crystalline oxalic acid in eight parts of hot water. After clarification with Norite, the filtered solution on cooling deposits crystals of the acid oxalate. About 5 g. of the salt remains in each 100 cc. of the mother liquor most of this can be obtained by evaporation and further crystallization. The amine is liberated from the pure oxalate with potassium hydroxide, distilled with steam, and purified as described above. When a known amount of amine is desired in water solution (as for optical resolution) a weighed amount of the (anhydrous) oxalate is decomposed and the amine is distilled quantitatively with steam. 

The successive crops of crystals are systematically recrystallized as follows, using Norite if necessary. About two-thirds of the first crop is dissolved in about three parts of water and the hot solution allowed to deposit crystals by slow cooling (Note 3). The liquor is filtered or decanted, the remainder of the first crop is dissolved in it, and the process of crystallization is repeated. The remaining crops are then similarly recrystallized in succession from the same liquor, the solution being evaporated to the appropriate volume before each crystallization. The final mother liquor is evaporated in stages and the viscous residue is united with that from the original crystallization. The various crops are systematically recrystallized from fresh water until pure... 

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