Preparation, III

The yield of 70 g. is obtained from benzyl cyanide, which boils over a 50 range prepared as described in preparation III (p. 9). Very pure benzyl cyanide will give a slightly higher yield, while commercial grades may give only 50 g. of jfr-nitro-benzyl cyanide and much oil. 

In a 5-I. round-bottom flask, fitted with a mechanical stirrer and reflux condenser, are mixed 1150 cc. of water, 840 cc. of commercial sulfuric acid and 700 g. of benzyl cyanide (preparation III, p. 9). The mixture is heated under a reflux condenser and stirred for three hours, cooled slightly and then poured into 2 1. of cold water. The mixture should be stirred so that a solid cake is not formed the phenylacetic acid is then filtered off. This crude material should be melted under water and washed by decantation several times with hot water. These washings, on cooling, deposit a small amount of phenylacetic acid which is filtered off and added to the main portion of material. The last of the hot water is poured off from the material while it is still molten and it is then transferred to a 2-1. Claisen distilling flask and distilled in vacuo. A small amount of water comes over first and is rejected about 20 cc., containing an appreciable amount of benzyl cyanide, then distils. This fraction is used in the next run. The distillate boiling i76-i89°/5o mm. is collected separately and solidifies on standing. It is practically pure phenylacetic acid, m. p. 76-76.5° it amounts to 630 g. (77.5 per cent of the theoretical amount). As the fraction which is returned to the second run of material contains a considerable portion of phenylacetic acid, the yield actually amounts to at least 80 per cent. 

Garrett, E. R. (1956), Prediction of stability in pharmaceutical preparations III. Comparison of vitamin stabilities in different multivitamin preparations. /. Am. Pharm. Assoc. Sci. Ed., 45,470-473. 

Q12 Pharmacological treatment of peptic ulcers aims to restore the balance between mucosal defence and mucosal damage by acid and pepsin in the stomach wall. The general mechanisms of drug action include (i) inhibition of acid secretion, (ii) neutralization of the acid with antacid preparations, (iii) eradication of H. pylori with antibiotics and (iv) enhancement of the mechanisms which protect the mucosa. 

Benzimidazol-2-yl-benoxazole derivatives of the current invention have also been prepared, (III), (4). 

In a previous study by the author spiro[benzo[c]thiophene-1-(3H), 4 -piperidine derivatives were prepared (III) and are described (2). 

Birner J, Garnet JR. Thimerosal as a preservative in biological preparations III factors affecting the concentration of thimerosal in aqueous solutions and in vaccines stored in rubber-capped bottles. ] Pharm Sci 1964 53 1424-1426. 

It is more difficult to prepare III-V semiconductors than the II-VI. Two sonochemical investigations reported on the preparation of these materials. The first paper details a safe method for the preparation of transition metal arsenides, FeAs, NiAs, and CoAs [142]. At room temperature, well-crystallized and monodispersed arsenide particles were successfully obtained under high-intensity ultrasonic irradiation for 4 h from the reaction of transition metal chlorides (FeCla, NiCl2, and C0CI2), arsenic (which is the least toxic arsenic feedstock) and zinc in ethanol. Different characterization techniques show that the product powders consist of nanosize particles. The ultrasonic irradiation and the solvent are both important in the formation of the product. 

Karo, S. (ed.). Organic Functional Group Preparations III Academic Press New York, 1972. 

Figure 2 SDS-PAGE or preparation I and II (100 and 2000 U/mL) as well as preparation III (250 and 5000 U/mL) using 5-20% gel and nonreducing conditions. Samples were boiled in sample buffer. Molecular weight markers are indicated by arrows on the left.

The chemical analysis consists of the following steps (i) Sample collection and storage (ii) Pretreatment and sample preparation (iii) Measurement (iv) Data processing and validation. Sample collection and storage are very critical steps in the whole procedure. Faults made during these steps cannot be corrected afterwards. Sample preparation must be taken into account in the calibration. The risk of contamination will increase with decreasing concentration of the analyte. Attention must be paid especially to contamination in the determination of ultra small amounts (p.p.b.-level). 

II NaCl-washed preparation. III MgCl2 washed preparation. 1 Untreated, 2 Treated with 0.1% EDC. Gels were stained with Coomassie Brilliant Blue R-250. Arrow heads, cross-linked product bands. 

In the J. Heyrovsk Institute we performed a detailed study of (a) M0O3 supported on siliceous mesoporous sieves of several types and (b) rhenium (VII) oxide supported on organized mesoporous aluminas in order to (i) verify positive effect of these supports on catalyst activity, (ii) to find out the most convenient way for catalyst preparation, (iii) to receive detailed information about their catalytic activity and selectivity, and (iv) to show the applicability of these catalysts in different types of metathesis reaction. 

A different method was utilized to prepare III (24) in order to avoid all possible doubt, resulting from the utilization of the Cbzo-glutamic anhydride, which reacts to give a mixture of isomers a and 7 (378,435). This method is based on the opening of the lactame bond of the pyrrolidone nucleus by treatment of 2-pyrrolidone-5-carboxylic acid and its amide with hydrogen chloride-saturated ethanol. 

---