By Miscellaneous Procedures

Minor routes to halogeno-l,5-naphthyridines are illustrated by the following examples. 

2-Chloro- gave 2-iodo- 1,5-naphthyridine (Nal, 50% HT, AcEt, 95°C, 8 h 47%) likewise, 4-chloro- gave 4-iodo-1,5-naphthyridine (68%).692 

---

Several miscellaneous procedures have been reported for the preparation of L-gulonic acid (47). 5-0-Benzoyl-l,3 2,4-di-0-ethylidene-D-glucitol (72) was oxidized388 with chromium trioxide to 73. After hydrolysis of 73, the L-gulose (45) formed was oxidized369,370 with bromine to 21. As noted in Section III,5b, 3,5 4,6-di-0-ethylidene-L-gu-lonic acid (50) was prepared from 3,5 4,6-di-0-ethylidene-D-gulitol (49) in 50-70% yield. By hydrolysis, 50 afforded333 21. 

A catalyst system159 consisting of a mixture of boron trifluoride, acetic acid and pyridine gives rapid and reproducible total hydroxyl analysis (silanol plus water) in a variety of silicone materials. This method avoids many of the interferences, empirical calibration and miscellaneous problems such as poor solubility, incomplete reaction and interfering siloxane cleavage associated with many earlier methods. Results obtained by this procedure compare well with results obtained by the lithium aluminium hydride procedure160. 

Amongst the miscellaneous procedures by which phenols have been derived may be mentioned the catalytic reduction of a cumene nuclear hydroperoxide with hydrogen and Pd/AljOj under a slight pressure for 5 hours at less than... 

Miscellaneous polysaccharides—This includes compounds that are undigestible, but which are not likely to be detected by the procedures usually employed in the analyses of foods for fiber content. Examples of such compounds are inulin, a water-soluble polysaccharide made up of fructose units and found in various roots and tubers such as the Jerusalem artichoke, and galactan, a galactose polysaccharide found in agar, a material obtained from seaweed. 

Miscellaneous Procedures. Most of the other procedures for the determination of —SH groups are variants of the processes indicated above. Of particular interest are the several amperometric titration procedures which, in effect, depend on mercaptide formation. Polarographic methods have also been used. An interesting submicro method for cystine by a Cartesian diver technique has recently been developed the method depends on the catalytic effect of —SS— groups on the decomposition of azide ion to nitrogen (78,94). The method cannot be applied to the direct determination of —SH groups. 

Experimental procedures have been described in which the desired reactions have been carried out either by whole microbial cells or by enzymes (1—3). These involve carbohydrates (qv) (4,5) steroids (qv), sterols, and bile acids (6—11) nonsteroid cycHc compounds (12) ahcycHc and alkane hydroxylations (13—16) alkaloids (7,17,18) various pharmaceuticals (qv) (19—21), including antibiotics (19—24) and miscellaneous natural products (25—27). Reviews of the microbial oxidation of aUphatic and aromatic hydrocarbons (qv) (28), monoterpenes (29,30), pesticides (qv) (31,32), lignin (qv) (33,34), flavors and fragrances (35), and other organic molecules (8,12,36,37) have been pubflshed (see Enzyp applications, industrial Enzyt s in organic synthesis Elavors AND spices). 

Although the use of barbiturates and miscellaneous sedatives and hypnotics for sedation has largely been replaced by the antianxiety drugs (see Chap. 30), they occasionally may be used to provide sedation before certain types of procedures such as cardiac catheterization or the administration of a local or general anesthesia Sedative doses usually given during daytime hours, may be used to treat anxiety and apprehension. Fhtients with chronic disease may require sedation, not only to reduce anxiety, but also as an adjunct in the treatment of their disease... 

This chapter discusses drug s used to treat urinary tract infections (UTIs) and certain miscellaneous drag > used to relieve the symptoms associated with an overactive bladder (involuntary contractions of the detrusor or bladder muscle). Structures of the urinary system that may be affected include the bladder (cystitis), prostate gland (prostatitis), the kidney, or the urethra (see Pig. 47-1). These drug s also help control the discomfort associated with irritation of the lower urinary tract mucosa caused by infection, trauma, surgery, and endoscopic procedures. 

Miscellaneous Reactions of Phosphines.- The role of chiral phosphines as ligands in the catalysis of reactions leading to the formation of chiral products has been reviewed.1111 A procedure for the determination of the enantiomeric excess in chiral phosphines has been developed, based on 13C n.m.r. studies of the diastereoisomeric complexes formed by phosphines with the chiral pinenyl nickel bromide complex. 111 Studies of the sulphonation of triphenylphosphine and of chiral arylphosphines have been reported in attempts to prepare water soluble ligands which aid... 

The end points of precipitation titrations can be variously detected. An indicator exhibiting a pronounced colour change with the first excess of the titrant may be used. The Mohr method, involving the formation of red silver chromate with the appearance of an excess of silver ions, is an important example of this procedure, whilst the Volhard method, which uses the ferric thiocyanate colour as an indication of the presence of excess thiocyanate ions, is another. A series of indicators known as adsorption indicators have also been utilized. These consist of organic dyes such as fluorescein which are used in silver nitrate titrations. When the equivalence point is passed the excess silver ions are adsorbed on the precipitate to give a positively charged surface which attracts and adsorbs fluoresceinate ions. This adsorption is accompanied by the appearance of a red colour on the precipitate surface. Finally, the electroanalytical methods described in Chapter 6 may be used to scan the solution for metal ions. Table 5.12 includes some examples of substances determined by silver titrations and Table 5.13 some miscellaneous precipitation methods. Other examples have already been mentioned under complexometric titrations. 

Methods for the A-acylation of similar heterocycles, such as simple thiazolidinethiones, have been reported since 1977, namely acyl chlorides in miscellaneous conditions,586 or carboxylic acids under DCC-activation.60,61 However the easiest and most effective method involves acyl chlorides or carboxylic anhydrides in the presence of an amine.47 Applying that procedure on carbohydrate scaffolds Rollin and co-workers62 reported the synthesis of diverse /V-acylated OZTs. The reactions were performed with good yields and the /V-selective acylation was ascertained by NMR— namely the thiocarbonyl 13C chemical shift (Scheme 41). Thanks to the dual nature of the carbanion drifting in the reaction,596 60 no competitive formation of the thioester, as mentioned by Plusquellec el al. in the case of benzothiazole, was observed. 

Part—I has three chapters that exclusively deal with General Aspects of pharmaceutical analysis. Chapter 1 focuses on the pharmaceutical chemicals and their respective purity and management. Critical information with regard to description of the finished product, sampling procedures, bioavailability, identification tests, physical constants and miscellaneous characteristics, such as ash values, loss on drying, clarity and color of solution, specific tests, limit tests of metallic and non-metallic impurities, limits of moisture content, volatile and non-volatile matter and lastly residue on ignition have also been dealt with. Each section provides adequate procedural details supported by ample typical examples from the Official Compendia. Chapter 2 embraces the theory and technique of quantitative analysis with specific emphasis on volumetric analysis, volumetric apparatus, their specifications, standardization and utility. It also includes biomedical analytical chemistry, colorimetric assays, theory and assay of biochemicals, such as urea, bilirubin, cholesterol and enzymatic assays, such as alkaline phosphatase, lactate dehydrogenase, salient features of radioimmunoassay and automated methods of chemical analysis. Chapter 3 provides special emphasis on errors in pharmaceutical analysis and their statistical validation. The first aspect is related to errors in pharmaceutical analysis and embodies classification of errors, accuracy, precision and makes... 

A small amount of solid may be dissolved in water and ammonium ion determined by the ion-selective electrode method, or miscellaneous colorimetric or titrimetric procedures (see Ammonia). Sulfate ion maybe determined by ion chromatography. 

Miscellaneous. A manometric technique utilizing a Warburg apparatus has been used to follow esterase activity. The carbon dioxide liberated from sodium bicarbonate by the fatty acids is measured (Willart and Sjostrom 1959). An agar diffusion procedure has been utilized for screening microorganisms for lipolyptic enzymes. The presence of lipase is indicated by clear zones in the turbid media (Lawrence et aL 1967). 

This author does not favor the use of static charge meters because their use is subject to operator diligence. It is a safer procedure to avoid the conditions which promote static charge accumulation as a matter of routine. Low ambient humidity is the chief contributing factor in the accumulation of hazardous static charges. In many desert areas (which seem to be favorites for ordnance work), the daytime ambient humidity is below 20% and in temperate regions, winter-time air, and indoor air, has likewise a low humidity. For this reason, also, air conditioned air, in the absence of artificial humidification, should be strictly controlled. In order to maintain a relatively safe humidity above 50% RH, the use of evaporative coolers is helpful in a desert environment. The matter of humidity control in pyrot processing plants was recently considered by Avrami et al (Refs 55 56) Miscellaneous Laboratory Hazards... 

Structural Steel - Use procedure in Section 19.3 to develop take-offs and cost. Break down by structures and pipe racks and don t forget to identify and estimate miscellaneous service ladders and platforms related to specific equipment items. 

CA s Directions for Abstractors and Section Editors is a 46-page booklet containing information on assignments, procedures, style, forms, abbreviations, nomenclature, notation, and numerous miscellaneous details, as well as a full discussion of the nature of the abstract desired. This booklet is indexed by subjects. Chemical Abstracts has a special 14-page set of Instructions for Abstracting Patents, and, for the sake of emphasis, the more important directions for abstracting are frequently distributed as a separate group in so-called Abstracted Directions. ... 

---