Solid reaction product filtering

The autoclave is cooled to room temperature, and the carbon dioxide is bled off. The solid reaction product is taken from the autoclave, pulverized, and dissolved in 1 1. of water at 50-60°. Ten grams of decolorizing carbon is added, and the mixture is stirred well and filtered to remove cadmium salts and carbon. The filtrate is heated to 80-90° and acidified with concentrated hydrochloric acid to pH 1 (Note 5). 2,6-Naphthalenedicar-boxylic acid precipitates. It is separated from the hot mixture by filtration. It is then suspended in 500 ml. of water at 90-95° (Note 5), separated by filtration, and washed successively with 300 ml. of water, 300 ml. of 50% ethanol, and 300 ml. of 90% ethanol. After being dried at 100-150°/150 mm. in a vacuum oven, the 2,6-naphthalenedicarboxylic acid weighs 42-45 g. (57-61%). It decomposes on a heated block at 310-313°. 

Then the cooled tube is wrapped in aluminum foil except for an area near the bottom of its neck, which is scratched with a glass cutter. The neck is snapped to open the tube, and the solid reaction product is removed and ground in a mortar. The powder is transferred to a 3-L beaker or Erlenmeyer flask and is stirred for 5 h with 1500 mL of deionized water. The mixture is allowed to settle for up to 3 h, then it is filtered through fluted filter paper. The solid residue... 

Finally, add an excess of concentrated hydrochloric acid slowly with stirring to the alkaline filtrate remaining from the original reaction product. As the solution becomes acid, the sulphonyl-aniline separates as a thick sticky syrup which, when stirred, rapidly crystallises. Cool the mixture in ice-water if necessary, and then filter off the solid product at the pump, wash well with water, and drain. Recrystallise from a mixture of 2 volumes of ethanol and i volume of water to prevent the sulphonyl-aniline from separating as an emulsion, allow the hot solution to cool spontaneously (with occasional stirring) until crystallisation starts, and... 

The reduction is effected exactly as in Procedure 8a but using 0.61 g (0.088 g-atom) of lithium. After the crude reaction product has been washed well on the filter with cold water, it is dissolved in ethyl acetate, the solution is filtered through the sintered glass funnel to remove iron compounds from the ammonia, and the filtrate is extracted with saturated salt solution. The organic layer is dried over sodium sulfate and the solvent is removed. The solid residue is crystallized from methanol (120 ml) using Darco. The mixture is cooled in an ice-bath, the solid is collected, rinsed with cold methanol, and then air-dried to give 12.9 g (85%), mp 129-132° reported for the tetrahydropyranyi ether of 3j5-hydroxypregn-5-en-20-one, mp 129-131°. 

The mixture was stirred at ice bath temperature for 2 hours, 1 ml of methanol was added and the mixture was filtered to remove insoluble impurities. Two milliliters of water were added to the filtrate and the pH was adjusted momentarily to pH 1.5, to effect removal of theenamine block, and then to pH 4.5 with triethylamine. After stirring for an additional hour at ice bath temperature the reaction product,7-(D-0 -phenylglycylamido)-3-chloro-3-cephem-4-carboxylic acid (zwitterion) precipitated from the reaction mixture as a crystalline solid. 

The reaction product mixture is a homogenous solution having a pH of about 6. It is evaporated under vacuum to a semisolid residue. To the residue are added 35 ml of water and a few drops of triethylamine to raise the pH to 8. The aqueous solution obtained thereby is extracted successively with 50 ml and 35 ml portions of ethyl acetate, the pH being adjusted to 2 at each extraction with hydrochloric acid. The extracts are combined, filtered, dried over sodium sulfate, stripped of solvent, and evaporated under vacuum. The product is 7-(N-carbobenzoxy-D-o -aminophenylacetamido)cephalosporanic acid in the form of a yellow-white amorphous solid weighing 1.10 g. 

A mixture of 20 g of 1 -bromo-3,5-dimethyladamantane, 75 ml of acetonitrile, and 150 ml of concentrated sulfuric acid was allowed to react overnight at ambient room temperature. The red reaction product mixture was poured over crushed ice, and the white solid which precipitated was taken up in benzene and the benzene solution dried over sodium hydroxide pellets. The benzene solution was filtered from the drying agent and evaporated to dryness in vacuo to yield 1 B.2 g of product having a melting point of about 97°C and identified by infrared spectrum as 1-acetamido-3,5-dimethvladamantane. 

The reaction product, which is a dark reddish-brown liquid, is poured or siphoned (Note 5) into 1.5 1. of water to which 50 cc. of a saturated solution of sodium bisulfite has been added (Note 6). The mixture is distilled with steam (Org. Syn. 2, 80) and the first portion of the distillate is collected separately to remove a small amount of unchanged nitrobenzene. It is necessary to collect about 12 1. of distillate in order to obtain all of the m-bromonitrobenzene. The yellow crystalline solid is filtered with suction and pressed well on the funnel to remove water and traces of nitrobenzene. The yield of crude product varies from 270-340 g. (60-75 Per cent °f the theoretical amount). It melts at 51.5-520 and boils at 117-118 79 mm. This product is satisfactory for most purposes. If a purer material is desired, the crude /w-bromonitrobenzene may be distilled under reduced pressure. The recovery on purification is about 85 per cent. Briihl recorded the b.p. as 1380/18 mm. and the m.p. as 56° for pure wz-bromonitrobenzene.1... 

Hydrolysis of methyl m-nitrobenzoate to m-nitrobenzoic acid. Place 90-5 g. of methyl m-nitrobenzoate and a solution of 40 g. of sodium hydroxide in 160 ml. of water in a 1-litre round-bottomed flask equipped with a reflux condenser. Heat the mixture to boiling during 5-10 minutes or until the ester has disappeared. Dilute the reaction mixture with an equal volume of water. When cold pour the diluted reaction product, with vigorous stirring, into 125 ml. of concentrated hydrochloric acid. Allow to cool to room temperature, filter the crude acid at the pump and wash it with a little water. Upon drying at 100°, the crude m-nitrobenzoic acid, which has a pale brownish colour, weighs 80 g. and melts at 140°. Recrystallisation from 1 per cent, hydrochloric acid affords the pine acid, m.p. 141°, as a pale cream solid the loss of material is about 5 per cent. 

Method 2. The procedure described under Benzenesulphonyl Chloride, Method 2 (Section IV,206) may be used with suitable adjustment for the difference in molecular weights between sodium p-toluenesulphonate (Section IV,30) and sodium benzenesulphonate. When the reaction product is poured on to ice, the p-toluenesulphonyl chloride separates as a solid. This is filtered with suction it may be recrystallised from hght petroleum (b.p. 40-60°) and then melts at 69°. 

After reaction, any solid residue was filtered off and the liquid product was separated by distillation into a bottoms product and a distillate that included unreacted Tetralin and low-boiling products from both the coal and the Tetralin. As tetralin breaks down under dissolution conditions to form mainly the tetralin isomer 1-methyl indan, naphthalene and alkyl benzenes (4) it was assumed that no compound with a higher boiling point than naphthalene was formed from the solvent, and the distillation to recover solvent was therefore continued until naphthalene stopped subliming. Some residual naphthalene remained in the bottoms product its mass, as determined from nmr and elemental analysis, was subtracted from the mass of bottoms product recovered and included in the amount of distillate recovered. It was assumed that all naphthalene present came from the Tetralin, not the coal. However, as the amount of tetralin reacted was 10 times the amount of coal this assumption appears reasonable. 

The use of the perchlorate as desiccant in a drybag where contamination with organic compounds is possible is considered dangerous [1], Magnesium perchlorate ( Anhydrone ) was inadvertently used instead of calcium sulfate (anhydrite) to dry an unstated reaction product before vacuum distillation. The error was realised and all solid was filtered off. Towards the end of the distillation, decomposition and an explosion occurred, possibly owing to the presence of dissolved magnesium perchlorate, or more probably to perchloric acid present as impurity in the salt [2]. 

Og, 22 mmol) was cooled in a dry ice - acetone bath for 15 minutes. After cooling, a 1.0M solution of Boron tribromide in methylene chloride (16.5g, 66 mmol) was added and the reaction was allowed to reach room temperature. After stirring for 18h, the solution was slowly added to 300mL water and stirred for several hours until a light solid could be filtered. The solid was washed with water and dried to give the product in 95% yield. 

Experimentally, the use of mixed acid for the nitration of aromatic substrates is very convenient. Reactions are often quenched by the addition of water, where the product usually precipitates. Solids are simply filtered from the acid liquors and oils are either separated or extracted into organic solvents. However, on an industrial scale, these mixed acid nitrations create environmental problems from air and water pollution (Sections 4.3.5 and 4.8.2). 

The way in which the active microzone is retained also depends on its relationship to the detector (Fig. 2.6) and the type of interaction with the analyte or its reaction product. If the microzone is an integral part of the probe, an additional support (usually a membrane) is often required, so contact with the sample is hindered to some extent. On the other hand, a microzone located in a flow-cell can be retained in various ways. Thus, if the microzone consists of a porous solid or particle, the flow-cell is simply packed with two filters in order to avoid washing out (e.g. see [21]). Too finely divided solids (viz. particle sizes below 30-40 pm) should be avoided as they require pressures above atmospheric level, which complicates system design and precludes use of microzones with a high specific surface. Placing a separation membrane in a flow-cell is... 

A 100-mL Schlenk flask is charged with a mixture of anhydrous FeCla (1.00 g, 7.89 mmol), KSPh (1.75 g, 11.83 mmol), [PPli4]Cl (1.48 g, 3.94 mmol), and sulfur (0.32 g, 9.86 mmol). Then 40 mL of acetonitrile is added with continuous stirring. The resulting reaction mixture is stirred at room temperature for 45 min. The solution is filtered to remove KCl and unreacted sulfur, and 100 mL of diethyl ether is added to the filtrate. On standing for some hours, the solution exhibits deposition of a black crystalline solid. The product is isolated by filtration, washed twice with diethyl ether, and dried in vacuo. Yield 1.57 g (68%). 

A reactor charged with 4-ethynylbenzoic acid (2.01 mmol) dissolved in dimethylacetamide was treated with 1-hydroxybenzotriazole (2.01 mmol) and /V.V -dicyclohexyl-carbodiimide (2.07 mmol) and stirred for 2 hours at ambient temperature. The mixture was then treated with (S)-(+)-decylalaninate (2.13 mmol) and stirred at ambient temperature for 3 hours and then at 120°C for a further 3 hours. The reaction was filtered, concentrated, and the residue purified by a silica gel chromatography using chloroform and ethyl acetate. After recrystallization from hexane 0.33 g of product was isolated as a crystalline solid. 

The progress of the reaction can be monitored by TLC by working up a sample of the reaction mixture filter through Celite, cool to 0°C, and acidify to pH 1 with 10% aqueous HCI. The solid that precipitates is isolated by filtration and dissolved in dimethylformamide (DMF) for TLC analysis on Merck precoated-silica gel 60 plates with methyl ethyl ketone-methanol-water (4 1 1) as eluent, developed by dipping in 5% sulfuric acid-ethanol and heated to 450°C (e.g., with a Bunsen burner). Rf values are 0.25 for fl-cyclodextrin, 0.5 for monotosylate and 0.65 for a second product, probably ditosylate. 

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