Detailed Syntheses

Various properties (3,4,5,15,16,18-32) as well as the morphology ( L iJL, 19.,23 33) of such copolymers were investigated in great detail. Synthesis of these block copolymers, while complex, is potentially not costly since materials and methods used in the manufacturing of polysiloxanes and polycarbonates can be used. 

The detailed synthesis of the IL s used here was described earlier (6). Two samples were prepared having R = butyl but the Al/cation ratio was 3/2 and 2 mol/mol. One sample each was prepared having R = ethyl, hexyl, octyl, and dodecyl for which the Al/cation = 2 mol/mol. 

The dimer [ In(NEt2)3 2] was synthesized by reaction of LiNEt2 with InCl. " It was characterized by NMR and mass spectrometry. Oddly, the detailed synthesis and stnicture... 

AB maleimide benzocyclobutene monomers and polymers have also been actively studied and developed by researchers at the Dow Chemical Co. The first AB maleimide type benzocyclobutene monomer prepared and polymerized by Kirchhoff was the benzocyclobutenyl maleamic acid 106 [6]. The detailed synthesis of 106 is shown in Fig 44. 

The synthesis of MCM-41 was carried out according to the following molar compositions of Si02 NaOH CTMABr Acid H20= 1 x y z 100, where Acid stands for HF or HC1, and molar ratios x, y, and z can be changed accordingly. A detailed synthesis procedure has been reported elsewhere [12]. For the hydrothermal stability studies, 0.5 g of the solid calcined at 550 °C for 10 h in air was tested in 60 g of boiling water in a plastic bottle for several days. 

The amount of MFI- and MCM-41-type material were estimated from XRD peak intensities. For the samples containing only small amounts of MFI, the presence of non-XRD detectable structures were identified for all samples by weak intensities in the infrared spectra near a frequency of 550 cm-1, which is characteristic for a skeleton bending mode for the MFI type samples [7]. The hydrothermal stability obtained also varied considerably for the samples, in the following, only three samples revealing the best hydrothermal stability will be discussed in detail. Synthesis and characterization data for the selected samples A, B and C, are summarized in Tables 1 and 2. The corresponding data for a siliceous pure MCM-41 sample synthesized by the same procedure [4,5], have been included for comparison reasons. 

The self-condensation of /3-keto esters and related compounds occurs under the influence of either acidic or basic catalysts and constitutes one of the earliest syntheses of pyran-2-ones (l883LA(222)l). It exemplifies a synthesis of type (ii) (Scheme 85). Ethyl acetoacetate, for instance, gives a mixture of 4,6-dimethyl-2-oxopyran-5-carboxylic acid and its ethyl ester other esters behave similarly (59RTC364). Decarboxylation of the pyrancarboxylic acid occurs at 160 °C in sulfuric acid. The formation of the pyranone proceeds through a 5-keto ester which is considered to result from attack of the enolic form of the ester on protonated ethyl acetoacetate (51JA3531). A detailed synthesis of the pyran-5-carboxylic acid is available <630SC(4)549). 

Tertiary phosphite complexes of platinum(O) can be prepared by the hydrazine reduction of PtCl2 P(OR)3 2 (equation 384), or by replacement of triphenylphosphine in Pt(PPh3)3 (equation 385).1233 Alternatively the complexes can be prepared from Pt(j73-C3H5)(r/5-Cp) and the phosphite.1268 Heteronuclear INDOR measurements show that 2/(PP) has a value of +81 Hz in Pt P(OMe)3 4. A detailed synthesis of Pt P(OEt)3 4 has been published from K2PtCl4 and triethyl phosphite with KOH (equation 386).1267 The product is obtained as colorless crystals which can be handled in air. 

The detailed synthesis procedure and textural properties (surface area, Sggy in m2 g-1 pore volume, V in ml g"1 and main pore diameter, d in nm), determined by nitrogen adsorption from 8.E.T. method have been published elsewhere (refs. 13-18) and are summarized in Table 1, where the surface acidity and basicity of supports are also collected. These values were determined by a spectro-photometric method described elsewhere (ref. 19), that allows titration of the amount (in tunol g 1) of irreversibly adsorbed benzoic acid (BA, pKa> 4.19), pyridine (PY, pka= 5.25) or 2,6-diterbutyl-4-methylpyridine (DTMPY, pKa 7.5) employed as titrant agents of basic and acid sites, respectively. Furthermore, the apparent rate constant values of different supports in the gas-phase skeletal isomerization of cyclohexene (CHSI), in Mmol atm"1 g"1 s-1, at 673 K, are also collected in Table 1, because these values are another way of measuring the stronger acid sites of supports (ref. 19). 

Qualifying a third party requires that detailed synthesis, analytical, and GMP information are provided to the third party. This is usually passed to the third party in a technology transfer package (see later). Eventually the third party is registered in the NDA as a supplier who has committed to meet an agreed analytical specification. For materials well back in the synthesis and for raw materials, including solvents, one may need no more than basic analytical release information—appearance, identity, purity (sometimes it may be necessary to set limits on specific impurities). 

A more detailed synthesis procedure for the supports used in this study is provided in chapter 4 and information on the strength of these supports as a function of synthesis conditions can be found in [4], Some general information about the colloidal filtration method can be found in [5,6],... 

There are several reviews referring to manzamine alkaloids [7,31-35]. In this chapter, we will review the structure and source of manzamine alkaloids including the large-scale preparation of manzamine alkaloids for preclinical evaluation. We also discuss the detailed synthesis and bioactivities of manzamine alkaloids. 

Several review articles and a comprehensive book already exist which describe the detailed synthesis of the miscellaneous organic donor molecules and the experimental procedures to obtain organic conducting salts [33]. Therefore, only a few introductory remarks concerning the principal crystal growth technique will be given here. 

Bis-salicylidene (or bis-salen) derivatives of 1,2-diaminocyclo-hexane are prepared by treatment of the diamine (or its tartrate salt) with an o-hydroxybenzaldehyde derivative and are used for asymmetric manganese-, cobalt- or chromium-catalyzed reactions. The most important ligand of this type is A(A -bis(3,5-di-terf-butylsalicylidene)-diaminocyclohexane (12), the detailed synthesis of which has been published. Another important ligand is the atropoisomeric derivative (13) (eq 21). ... 

Detailed synthesis procedures for supported Ru (4) and Co (5, 41) catalysts have been reported previously. These catalysts were prepared by incip-... 

A more detailed synthesis of 4-nitrophenyl-, 2-naphthyl-, 2-phe-nanthryl-, 9-anthryl-, and 2-anthraquinonyl-substituted cobalt(III) sarcophaginates starting from the corresponding methylarylketones was reported in Ref. 137. 

Traylor and Singer (1967) have provided a detailed synthesis of the diazonium salts XIX and XX. Compound XIX has been used as an affinity label for acetylcholinesterase on erythrocyte membrane (Wofsy and Michaeli 1967) and for the cholinergic receptor from eel electroplax (Changeux et al. 1967). XX has been used for the modifica-... 

More recently, Rokach and Zamboni have reported the first stereospecific total synthesis of both the natural (5S)- and unnatural (5/ )-isomers of the 5-HETEs. The key to these syntheses, outlined in Schemes 3.3 and 3.4 was the use of the two enantiomeric aldehydes, (S)-21b and (/ )-21b, containing the asymmetric center which becomes C-5in the final products. The detailed synthesis of these key intermediates, both obtained from 2-deoxy-D-ribose, will be presented fully in Section 3.B... 

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