Preparative procedures

This section contains a brief description of the procedures for the synthesis of parent perimidinespirocyclohexadienone la (R = H) and some of its derivatives. 

A solution of 1,8-naphthylenediamine (4.74 g, 30 mmol) and 2,6,-di-fert-butyl-1,4-benzoquinone (6.6 g, 30 mmol) in propanol (10 ml) was refluxed for 5 h, then 

To a solution of la (R = H) 1.8 g, 5 mmol) and methyl iodide (2.84 g, 20 mmol) in dimethyl sulfoxide (10 ml), K2C03(6.9 g, 50 mmol) was added. The mixture was stirred for 10 h at room temperature and then poured into water (100 ml). The precipitate was filtered off, washed with water, dissolved in chloroform (10 ml), and passed through a column filled with A1203. The solvent was removed and a dark oily residue solidified on treatment with hexane. After two crystallizations from heptane, 1.12 g (yield 60%) of l-methyl-2,3-dihydro-2-spiro-4 -(2, 6 -di- fert-butylcy clohexadien-2, 5 -onc)pcrimidine were obtained as yellow needles mp 179-180°C. 

A mixture of 1,8-naphthalenediamine (3.48 g, 22 mmol), 2-tert-butyl-1,4-naphthoquinone (3.21 g, 15 mmol) and p-toluenesulfonic acid (50 mg) was melted together at 165-170°C for 4 h, cooled to room temperature and dissolved in chloroform (20 ml). The solution was passed through a column (40 x 3.5 cm) filled with A120 3. The column was washed with chloroform-hexane (1 3) and the fraction of orange color collected. After evaporation of the solvent, dark-yellow crystals of 2,3-dihydro-2-spiro-4 -[(4H)-2 -fert-butlnaphthalen-l -one]perimidine (2.06 g, yield 47.8%) were obtained, mp 211-213°C (after recrystallization from methanol and heptane). 

A solution of 5-amino-4-chloro-2,6,8-trimethylquinoline (0.22 g, 1 mmol) and 2,6-di-tert-butyl-4-aminophenol (0.35 g, 1.6 mmol) in o-xylene (5 ml) was refluxed for 3 h, then cooled to room temperature, diluted with chloroform (5-7 ml) containing 1 ml of saturated water solution of ammonia and allowed to stand 

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Most chromium-based catalysts are activated in the beginning of a polymerization reaction through exposure to ethylene at high temperature. The activation step can be accelerated with carbon monoxide. Phillips catalysts operate at 85—110°C (38,40), and exhibit very high activity, from 3 to 10 kg HDPE per g of catalyst (300—1000 kg HDPE/g Cr). Molecular weights and MWDs of the resins are controlled primarily by two factors, the reaction temperature and the composition and preparation procedure of the catalyst (38,39). Phillips catalysts produce HDPE with a MJM ratio of about 6—12 and MFR values of 90—120. 

Theoretical and applied aspects of microwave heating, as well as the advantages of its application are discussed for the individual analytical processes and also for the sample preparation procedures. Special attention is paid to the various preconcentration techniques, in part, sorption and extraction. Improvement of microwave-assisted solution preconcentration is shown on the example of separation of noble metals from matrix components by complexing sorbents. Advantages of microwave-assisted extraction and principles of choice of appropriate solvent are considered for the extraction of organic contaminants from solutions and solid samples by alcohols and room-temperature ionic liquids (RTILs). 

Comparing results obtained by concerned decomposition techniques with the data certified (recommended), the two-stage microwave sample preparation procedure is preferable. 

We are indebted to Dr. W. Novis Smith, formerly with Foote Mineral Company, and now with Stauffer Chemical Company, Dobbs Ferry, New York, for supplying the general preparative procedure which we have adapted to the laboratory-scale preparation described here. 

The Hiickel rule predicts aromaticity for the six-7c-electron cation derived from cycloheptatriene by hydride abstraction and antiaromaticity for the planar eight-rc-electron anion that would be formed by deprotonation. The cation is indeed very stable, with a P Cr+ of -1-4.7. ° Salts containing the cation can be isolated as a product of a variety of preparative procedures. On the other hand, the pK of cycloheptatriene has been estimated at 36. ° This value is similar to those of normal 1,4-dienes and does not indicate strong destabilization. Thus, the seven-membered eight-rc-electron anion is probably nonplanar. This would be similar to the situation in the nonplanar eight-rc-electron hydrocarbon, cyclooctatetraene. 

The low molar ratio of the final UF-resin is adjusted by the addition of the so-called second urea, which might also be added in several steps [16-18]. Particular care and know-how are needed during this acid condensation step in order to produce resins of good performance, especially at the very low molar ratios usually in use today in the production of particleboard and MDF. This last reaction step generally also includes the vacuum distillation of the resin solution to the usual 63-66% solid content syrup in which form the resin is delivered. The distillation is performed in the manufacturing reactor itself or in a thin layer evaporator. Industrial preparation procedures are usually proprietary and are described in the literature in only a few cases [17-19]. 

In the literature, various other types of resin preparation procedures are described, e.g. yielding uron structures [20-22] or triazinone rings in the resins [23,24]. The last ones are formed by the reaction of urea and an excess of formaldehyde under basic conditions in the presence of ammonia or an amine, respectively. These resins are used to enhance the wet strength of paper. 

The reactivity of a resin at a certain molar ratio F/U or F/(NH2>2 is mainly determined by its preparation procedure and the quality of the raw materials... 

The standard requires documented procedures to be prepared consistent with the requirements of this international standard, but what does this mean Preparing procedures consistent with the requirements of the standard means preparing those procedures where the standard requires them. Outside ISO 9001, ISO/TS 16949 does not use the same wording to require procedures. In some clauses it requires a process and in others it requires methods or a methodology or a system. Although systems are not procedures, procedures are not processes and methods are not necessarily procedures, systems, or processes. Some methods, however, will inevitable need one or more procedures. By including systems, methods, and processes, the standard now requires 43 documented procedures directly. 

Prepare procedures to control these tasks and the interfaces between them. 

Prepare procedures for the conduct of design verification activities. 

Prepare procedures for the preparation and maintenance of design and development plans. 

Prepare procedures for creating speciality plans covering reliability, safety, environmental engineering, etc. 

Prepare procedures governing the construction of models for use in proving the design. 

Once the make or buy decision has been made, control of any purchasing activity follows a common series of activities, which are illustrated in Figure 6.2. There are four key processes in the procurement cycle for which you should prepare procedures ... 

Prepare procedures for purchasing those products and services, the quality of which affects end product quality. 

Prepare procedures and standards that govern the specification of items to be purchased. 

Prepare procedures for assessing your subcontractors and suppliers. 

Prepare procedures for producing and maintaining subcontract requirements and letting tenders. 

Prepare procedures for evaluating tenders and selecting subcontractors. 

Prepare procedures covering the planning of subcontractor control activities. 

Prepare procedures for inspecting customer supplied product and notifying the customer of any problems. 

Prepare procedures for planning production of product lines, batched and single products. 

Prepare procedures for providing instructions governing production activities where necessary. 

Prepare procedures for provisioning tools, equipment, and facilities needed for production. 

Prepare procedures for inspecting and testing incoming goods. 

Prepare procedures for controlling the calibration of measuring devices. 

Prepare procedures controlling the development and maintenance of software used in measurement systems. 

Prepare procedures for controlling these quarantine areas. 

Prepare procedures for the analysis, investigation, and determination of the causes of potential and actual deviation including the formation of diagnostic teams where necessary. 

Prepare procedures for reporting the results of the analyses to management. 

Prepare procedures for evaluating the effectiveness of training and recording the results. 

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