Cooling adding

The presence of acetanilide in these residues may be confirmed by boilin the residue for two to three minutes with HCl, and when cool, adding a few drops of 0 5 per cent, of chlorinated lime solution, in such a manner that the liquids do not mix. A fine blue colour results if acetanilide be present. 

An alternative procedure involves the release of the fatty acids by alkaline hydrolysis (saponification) by refluxing the extracted sample with dilute alcoholic potassium hydroxide for 1 h. After cooling, adding water and acidifying, the fatty acids are extracted into diethyl ether. The methyl esters can then be prepared by treatment with diazomethane, which may also be used directly on free fatty acids. Saponification is less satisfactory, because it is a lengthy procedure and often results in the loss of lipid components. 

For its prepn were melted together 2 pts of nitre with 1 pt of K carbonate and, when the mass cooled, adding to 4% ps of it 1 pt of sulfur. This pdr was claimed to be no less than 8% times quicker than the best common BkPdr, More details are in Ref Ref Davis (1943), 31... 

The purity of a sample of sulphur monochloride may be determined by heating with aqueous sodium hydroxide (2N) for four hours in a long-necked flask on a water-bath and, after cooling, adding a few c.c. of 30 per cent, hydrogen peroxide. The mixture is then reheated for not more than half an hour, slightly acidified with nitric acid, and diluted to a known volume. The chlorine may then be estimated volumetrically and the sulphur gravimetrically in aliquot portions.8... 

Tris[2-thienyl] Telluronium Bromide3 2.2 g (4.8 mmol) of bis[2-thienyl] tellurium dibromide are added to a Grignard solution prepared from 1.7 g (10 mmol) of 2-bromothiophene in 50 ml of diethyl ether. The mixture is heated under reflux for 2 h, cooled, added to 15 ml of water, and filtered. The filter cake is washed with water and dried in a vacuum dessicator. The dry product is extracted with a large volume of methanol and the product precipitated by concentration of the extract m.p. 244° (253° corrected). 

Philadelphia, Pa, 1821, by triturating in a warm mortac 3 parts by wt of nitre, two of carbonate of potash and one of flower of sulfur. Its effects, when fused in a ladle and then set on fire, were very great. The whole of the melted material exploded with an intolerable noise, and the ladle disfigured, as if it had received a strong blow downwards, it was three times quicker dian common BkPdr A similar powder was manufd by S, Guthrie, Jr and sold in 1930 s in this country. He proposed, however, another powder, which he claimed to be superior to the above mixture. For its prepn were melted together 2 pts of nitre with 1 pt of K carbonate and, when the mass cooled, adding to 4)4 ps of it 1 pc of sulfur. This pdr was claimed to be no less than 8)4 times quicker than the best common BkPdr, More details are in Ref Ref Davis (1943), 51... 

A mixture of homoveratric acid (49 g), anhydrous sodium acetate (20.5 g) and acetic anhydride (83 mL) was refluxed for 4 hours, cooled, added to 500 mL. of ice-cold water and stirred for 15 minutes. The resulting reddish bottom layer was separated and retained. The remaining aqueous layer was extracted with two 100 mL. quantities of toluene, and the toluene extracts were combined with the reddish liquid and washed successively with five 100 mL. quantities of IN sodium hydroxide solution, followed by two 100 mL. quantities of water. The washed product was then filtered through a plug of glass wool and fractionally distilled to remove the toluene and water impurities. The product, 3,4-dimethoxyphenylacetone, was collected at 115°C to 125°C at about 0.4 mm Hg. This product was a pale yellowish oil and was obtained in a yield of 16 g (33% of theoretical yield). 

Figure 2. Methods of achieving supersaturation in high temperature solutions ABC, slow cooling AD, evaporation EF, thermal gradient transport. (From Ref. 2.).

A simpler but more costly procedure - involves dissolving triphenylcarbinol in acetic anhydride, cooling, adding 48% HBF4, followed by a benzene solution of tropilidene (with cooling) and then ether as precipitant. 

Acid amides may be easily saponified by dissolving in concentrated sulphuric acid, cooling, adding sodium nitrite, and then gradually heating,1 e.g. ... 

Blanc reaction. In carrying out the reaction of p-bromotoluene with formaldehyde and a Lewis acid catalyst to obtain the isomeric chloromethyl derivatives for use in a synthesis of methylcholanthrene, Fieser and Seligman18 fused a mixture of anhydrous zinc chloride with 1% of aluminum chloride and let it cool, added p-bromotoluene and paraformaldehyde, and passed a slow stream of hydrogen chloride into the mixture while heating it at 45-50° for 18 hrs. Use of the special catalyst increased the yield about threefold over that obtained with zinc chloride alone. 

Add water phase to oil phase while stirring. Stir to cool, adding triethanolamine at 60°C and perfuming at 40°-50°C. 

Bed Salve, Red lead, 1 pound bees -wax and resin, of each 2ounces linseed and sweet oils, of each 3 table-spoonfuU spirits of turpentine, 1 tea-spoonful melt all, except the first and last, together, then stir in the lead and stir until cool, adding the tuqjentine. Good for all inflamed sores,... 

Start to add the continuous monomer and initiator feeds to go in over 4 h at a steady rate. Monitor temperature and reflux continuously, especially in the early stages of the reaction. Slow the feed of monomer if reflux is excessive or temperature cannot be maintained at 80 to 85°C. Ensure that the agitation is sufficient at all times to give a small vortex that blends in added monomer and condenser return smoothly but does not create foam or splashing. When feeds are complete, add final initiator and allow temperature to rise to 90 2°C (heat if necessary). Hold for 20 min, then cool, adding the dibutyl phthalate at about 65°C and the preservative at 35°C or less. 

Frankland by the action of zinc amalgam on amyl iodide in a sealed tube, cooling, adding potassium and reheating, obtained a colourless liquid which he regarded as free amyl CioHn. By the action of zinc and water on amyl iodide he obtained what he regarded as amyl hydride (CioHn)H. In the first reaction some amylene CiqHio was obtained, as ethylene was in the reaction with ethyl iodide. 

Ice-cooled added dropwise during 20 min. below 10 to a mixture... 

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