General procedure ii

The general procedures for the preparations of half-esters of diols are not usually very efficient in that both unreacted diol and diester are present along with the desired half-ester. Unfortunately, the present example is no exception but is included as an illustration of the type of results that can be expected under these circumstances. The diol employed for this reaction is prepared in Chapter 5, Section II. 

Alkylation of Compound 1 with Chiral Tin(II) Enolate 2 General Procedure ... 

Another general procedure to prepare gold(II) complexes consists of substitution reactions on gold(II) derivatives. Halide ligands can be substituted by neutral donor ligands2025-2032 such as... 

A very recent addition to the already powerful spectrum of microwave Heck chemistry has been the development of a general procedure for carrying out oxidative Heck couplings, that is, the palladium)11)-catalyzed carbon-carbon coupling of arylboronic acids with alkenes using copper(II) acetate as a reoxidant [25], In a 2003 publication (Scheme 6.6), Larhed and coworkers utilized lithium acetate as a base and the polar and aprotic N,N-dimethylformamide as solvent. The coupling... 

Potter and co-workers 301) determined reducing sugars in plant materials by reducing copper(II) in alkaline solution to insoluble cuprous oxide and then measuring the excess copper in the filtrate. Mitschell248) conducted further studies on this method. Christian and Feldman 19) have described general procedures for the indirect determination of glucose and of protein. It is anticipated that in the future, we will see many more applications of atomic absorption spectroscopy to the indirect determination of nonmetals. 

Domino-Heck Reactions-General Procedure 5.6 mg (25 pmol) of palladium(II) acetate and 55 pmol of the arsine ligand were dissolved in 3 ml of dry dimethyl formamide and the solution was stirred at 65°C (40°C for trimethylsilylacetylene) for 15 mitt Then, 127 mg (1.35 mmol) N-Benzoyl-2-azabicyclo[2.2.1]hept-5-en-3-one, 1 mmol of the aryl compound. Four hundred and eighty-eight microliters (3.50 mmol) of triethylamine, and 3.00 mmol of the phenylacetylene (or silylmethyl-acetylene) were added rapidly in one portion. The mixture was heated at the same temperature for 24 h. After cooling down to room temperature 50 ml of brine were added, the reaction mixture was extracted with ethyl acetate and dried over MgSO. The solvent was evaporated, the residue purified by column chromatography (n-Hexan-Ethyl acetate 4 1). 

Concerning more general application of mercury electrode in the studies on com-plexation equilibria, one should mention the paper by Jaworski et al. [59], who have investigated oxidation of mercury microelectrode in solutions with thiocyanates without any background electrolyte added. In the experiments, normal pulse voltammetry and staircase voltammetry were used. The authors have developed a general procedure for the determination of the stability constants, based on the data taken from the voltammograms. They have applied it to the analysis of Hg(II)-SCN complexes. 

Other alkyl chlorides may be prepared by this general procedure.12 The following yields are obtained with some of the common alcohols, used in the molecular proportions given under the procedure ii-propyl chloride, 55-61 per cent iso-propyl chloride, 70-76 per cent sec.-butyl chloride, 60-65 Per cent 2-chloropentane, 60-70 per cent. 

A stable, readily soluable platinum ir-vinyl alcohol complex has now been synthesized and well characterized. Initially, this compound, chloro(acetylacetonato)(ir-ethenol)platinum(II) (45), was synthesized from the ir-ethylene compound (43) via a vinyl trimethylsilyl ether complex (44) using the same general procedure employed in the synthesis of (41) and (42) (44). 

Solutions of these metals in liquid ammonia effect (i) the reduction of a range of functional groups such as carbonyl and acetylenic and also conjugated and aromatic systems, and (ii) cleavage of benzyl and allyl ethers and thioethers. These reactions are usually carried out by the general procedure of adding the metal to a solution of the substrate in liquid ammonia to which dry methanol or ethanol or t-butanol has been added to provide a ready proton source (alcohols are more acidic than ammonia).34... 

A general procedure for regioselective synthesis of chlorins from porphyrins is described in Ref. [240]. The method is based on the experimental evidence that certain substituents (e.g. vinyl, acetyl, formyl) direct the photoreduction to the site of the ring to which they are attached. As an example, the photochemical synthesis of zinc(II) vinylchlorins from the corresponding porphyrins can be demonstrated (R = H, CH3, C2H5, C2H4COOCH3)... 

The above example (Schemes 2.9 and 2.10) illustrates a potentially general procedure (i) identify unexpected products (ii) consider mechanistic explanations (iii) modify reaction conditions (in this case using catalysts or inhibitors) to optimise the yield of desired products, and to test mechanistic deductions. Additional and more direct supporting evidence for radical intermediates is given in Chapter 10. 

Appearance of solution Carry out this test as directed in the general procedure (2.2.1), solution S is clear and not more intensely colored than reference solution B6 (Method II in the general procedure (2.2.2)). 

Heavy metals—Carry out this test as directed in the general procedure (231), Method II, 0.002%. 

A more generally useful procedure may be developed by preparing the acid chloride according to Procedure II and conducting the cyclization as in Procedure III. 

The Chemical Weapons Convention (CWC) provides sampling and analysis as a tool for verification. General procedures to use sampling and analysis are outlined under the general rules of verification in the Verification Annex (VA) Part II paragraph 52-58, special provisions concerning different types of inspections are given in various parts of the VA. 

All compounds listed in Table II (except 2i) were prepared by this general procedure. Other suitable catalysts were 5% Pd/C and 5%Pd-Al203. 

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