Stirred continuous

Place 50 g. of o-chloronitrobenzene and 75 g. of clean dry sand in a 250 ml. flask equipped with a mechanical stirrer. Heat the mixture in an oil or fusible metal bath to 215-225° and add, during 40 minutes, 50 g. of copper bronze or, better, of activated copper bronze (Section 11,50, 4) (1), Maintain the temperature at 215-225° for a further 90 minutes and stir continuously. Pour the hot mixture into a Pyrex beaker containing 125 g. of sand and stir until small lumps are formed if the reaction mixture is allowed to cool in the flask, it will set to a hard mass, which can only be removed by breaking the flask. Break up the small lumps by powdering in a mortar, and boil them for 10 minutes with two 400 ml. 

Method 2. In a 500 ml. round-bottomed flask, equipped with a reflux condenser, place 20 5 g. (20 ml.) of anUine, 21 5 g. (20 ml.) of acetic anhydride, 21 g. (20 ml.) of glacial acetic acid, and 01 g. of zinc dust (1), Boil the mixture gently for 30 minutes, and then pour the hot Uquid in a thin stream into a 1 Utre beaker containing 500 ml. of cold water whilst stirring continually. When cold (it is preferable to cool in ice), filter the crude product at the pump, wash with a Uttle cold water, drain well and dry upon filter paper in the air. The yield of acetaniUde, m.p. 113°, is 30 g. It may be recrystaUised as in Method 1 aflFording 21 g, of pure acetaniUde, m.p. 114°. 

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... 

Potassium biiodate [13455-24-8] M 389.9. Crystd three times from hot water (3mL/g), stirred continuously during each cooling. After drying at 100° for several hours, the crystals are suitable for use in volumetric analysis. 

In a 3-I. round-bottomed, three-necked flask fltted with a liquid-sealed mechanical stirrer, a thermometer, and a 500-cc. separatory funnel are placed 1700 cc. of dry ben2ene and 160 g. (1.2 moles) of powdered, anhydrous aluminum chloride (Note i). The mixture is cooled to 10° by means of an ice-water bath and maintained at 10-20 during the addition of a solution of 120 g. (0.58 mole) of benzalacetophenone (Note 2) (Org. Syn. Coll. Vol. I, 71) in 300 cc. of dry benzene. This addition requires about thirty minutes. The cooling bath is then removed and stirring continued at room temperature until all the dense, yellow precipitate formed at first has gone into solution (Note 3). The reaction is complete after stirring for an additional hour. 

A solution of 7.2 g of sodium borohydride (analyzing at 87 % purity) in 300 ml of pyridine is added dropwise, with vigorous stirring, over 7 hr to a solution of 50 g of pregnane-3,11,20-trione in 100 ml of pyridine and 18 ml of water. The temperature is kept at 18-20°. The stirring at this temperature is continued for another 2 hr, after which the reaction mixture is poured slowly into dilute hydrochloric acid (575 ml of cone hydrochloric acid in 5.2 liters of water) and the stirring continued for 1 hr. The precipitate is filtered, washed with... 

The rhodium catalyst (46 mg) is dissolved in acetone (10 ml) in a microhydrogenation apparatus which is then flushed three times with deuterium gas. After stirring the solution in an atmosphere of deuterium for about 1 hr the deuterium uptake ceases and constant pressure is attained. 5a-Cholest-2-ene (136, 19.5 mg) is added and the stirring continued until deuterium uptake ceases (about 3/4 hr). The solvent is evaporated to dryness and the residue is extracted with hexane and the resulting solution filtered through a small alumina column (3 g, activity 111). Evaporation of the hexane gives 2, 3 -d2-5oc-cholestane (137) 18 mg, 92% mp 78-79° isotope composition 94%d2,5%d, andl%do. ... 

B) Acylation of 6-Aminopenicillanic Acid To a solution of the aryl halocarbonyl ketene (0.1 mol) in methylene chloride (sufficient to provide a clear solution and generally from about 5 to 10 ml per gram of ketene) there is added the proper alcohol RjOH (0.1 mol), in this case 5-indanyl alcohol. The reaction mixture is maintained under an atmosphere of nitrogen and stirred for a period of from 20 minutes to 3 hours, care being taken to exclude moisture. The temperature may range from about -70° to about -20°C. The infrared spectrum of the mixture is then taken to determine and confirm the presence of the ketene ester. A solution of 6-aminopenicillanic acid-triethylamine salt (0.1 mol) in methylene chloride (50 ml) is added and the mixture stirred at -70° to -20°C for 10 minutes. The cooling bath is then removed and the reaction mixture stirred continuously and allowed to warm to room temperature. 

Stage 4 Preparation of 1-l2-Phenyi-2-Methoxyl -Ethyi-4-[3-Phenyl-3-Hydroxypropyl] -Piperazine Dihydrochioride - In a double-neck flask equipped with a thermometer and a mechanical stirrer, there is placed in suspension in 800 ml of methanol, 233 grams of 1-[2-phenyl-2-methoxy]-ethyl-4-[2-benzoyl-ethyl]-piperazine dihydrochioride (0.55 mol). It is cooled to approximately 5°C, and 46 grams of NaOH pellets dissolved in 80 ml of HjO are added. When the temperature is about 5°C, one addition of 29,2 grams of sodium borohydride in 40 ml HjO is made. The ice-bath is then removed and stirring continued at ambient temperature for 6 hours. 

Chlorine gas was gradually passed into 660 parts of benzene contained in a lead-lined reaction vessel until 890 parts of the gas had been absorbed. The mixture was stirred continuously and the temperature maintained at 15°C to 20°C. 

A solution of 32 g (030 mol) phosgene in 200 ml benzene is added dropwise at 30°C to a stirred soiution of 53.5 g (032 mol) 3-o-toloxy-13-Pfopanediol in 400 ml benzene. The mixture is stirred for an hour after the addition is completed, and a solution of 39 g of dl-methylaniline in 100 ml benzene is then added, and stirring continued for a half-hour. Ice water (about one-third volume) is then added, and the benzene layer formed is separated and stirred with 500 ml concentrated ammonia at 5°Cfor six hours. The precipitated solid (weighing about 55 g) is recovered and recrystallized from water. The product thus obtained in a yield of about 53 g is 3-(o-toloxy)-2-hydroxypropyl carbamate it is a crystalline solid melting at about 93°C, and having a lower water-solubility and higher oil-solubility than 3-o-toloxy-13-propanediol. 

To the aqueous suspension of the palladized charcoal catalyst thus obtained are added 20.8 kg of 3-cyano-pyridine (96% purity) and then are added 70 liters of a hydrochloric acid solution prepared by diluting 30 liters of 36% HCI with 40 liters of water. This represents approximately 1.75 mols of HCI for each mol of 3-cyano-pyridine. The suspension is maintained at 10° to 15°C and stirred continuously while introducing a current of hydrogen at a pressure of 3 to 5 psi. When absorption of hydrogen ceases and the 3-cyano-pyridine is completely reduced, the reaction mixture is filtered to remove the catalyst. 

To a batch of approximately 10 liters of filtered broth is added 150 grams of activated charcoal. The mixture is stirred continuously for about 5 minutes and is then filtered. 

N-Acetylation of Kasugamycinic Acid (9a). A solution of kasugamycinic acid (225 mg.) dissolved in 10 ml. of water was treated with acetic anhydride (0.3 ml.) under cooling sodium bicarbonate was used to keep the pH 7.2 and stirring continued for 30 minutes. The reaction product was passed through Dowex 50W-X2 (H form) and the column was washed with water. The combined filtrate was subjected to lyophilization to afford 234 mg. of a crude N-acetyl derivative. Its infrared spectrum showed strong absorptions at 1740 cm-1 characteristic of oxamic acid group. The N-acetyl derivative (178 mg.) was treated with 40 ml. 

Preparation ofpure potassium hydrogeniodate. Dissolve 27 g of potassium iodate in 125 mL of boiling water, and add a solution of 22 g of iodic acid in 45 mL of warm water acidified with six drops of concentrated hydrochloric acid. Potassium hydrogeniodate separates on cooling. Filter on a sintered-glass funnel, and wash with cold water. Recrystallise three times from hot water use 3 parts of water for 1 part of the salt and stir continuously during each cooling. Dry the crystals at 100 °C for several hours. The purity exceeds 99.95 per cent. 

Add cautiously (FUME CUPBOARD), and with constant stirring, 10 mL of the ammonium citrate solution this will prevent the precipitation of metals when, at a later stage, the pH value of the solution is increased. Then add 10 mL of the 20 percent ascorbic acid, and adjust to pH 4(BDH narrow-range indicator paper), by the cautious addition of concentrated ammonia solution down the side of the beaker while stirring continuously. Then add lOmL of the 50 per cent potassium cyanide solution (CAUTION ) and immediately adjust to a PH of 9-10 (BDH indicator paper) by the addition of concentrated ammonia solution. 

Jha and Bhowmick [51] have reported the development and properties of thermoplastic elastomeric blends from poly(ethylene terephthalate) and ACM by solution-blending technique. For the preparation of the blend the two components, i.e., poly(ethylene terephthalate) and ACM, were dried first in vacuum oven. The ACM was dissolved in nitrobenzene solvent at room temperature with occasional stirring for about three days to obtain homogeneous solution. PET was dissolved in nitrobenzene at 160°C for 30 min and the rubber solution was then added to it with constant stirring. The mixture was stirred continuously at 160°C for about 30 min. The blend was then drip precipitated from cold petroleum ether with stirring. The ratio of the petroleum ether/nitrobenzene was kept at 7 1. The precipitated polymer was then filtered, washed with petroleum ether to remove nitrobenzene, and then dried at 100°C in vacuum. 

The mixed solution obtained was then placed in a syringe and allowed to drop into a sterile 0.2M CaCli solution that was stirred continuously. Alginate drops solidified upon contact with CaCh, forming beads and thus entrapping bacteria cells. The beads were allowed to harden for 30 minutes at 37 C and then washed with sterile saline solution to remove excess calcium ions and untrapped cells. 

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