Synthesis monohydrate

C, b.p. 205°C, forms monohydrate m.p. 58°C. Prepared from diacetoneamine and propanone or by passing NH3 gas into pro-panone containing fused CaCl2. Decomposes to phorone and ammonia, reduced to lelra-melhyl-3-hydroxypiperidine. Used in the synthesis of benzamine hydrochloride. 

Meclizine Hydrochloride. Pipera2ine Antivert, and Bonine are trade names for mech2ine dihydrochloride monohydrate [31884-77-2] (20). It is a white or slightly yellowish crystalline powder with a slight odor, no taste, and a melting point of 217—224°C. The hydrochloride is practically insoluble in water and ether. It is freely soluble in chloroform, pyridine, methylacetamide, and mild acid alcohol—water mixtures, and is slightly soluble in dilute acids or alcohol. See Reference 16 for synthesis. 

Pterin, 6,7,7-trimethyl-7,8-dihydro-bacteriostatic activity, 3, 325 Pterin, 5,6,7-trimethyl-5,6,7,8-tetrahydro-dihydrochloride monohydrate X-ray analysis, 3, 281 Pterin-6-carbaldehyde, JV -acetyl-synthesis, 3, 312... 

Constitution. Comparison of the empirical formula of the three alkaloids, and the fact that jatrorrhizine and columbamine each stands to palmatine in the relation of a monohydric phenol to its methyl ether, makes it clear that the only difference between jatrorrhizine and columbamine must be in the position of the free hydroxyl group. The method by which this point was settled is described in dealing with the two tetrahydro-derivatives of these alkaloids (p. 291). The constitution of palmatine (XXV R = R = Me) is dealt with under tetrahydropalmatine, but it is still necessary to describe the complete synthesis of this alkaloid via oxypalmatine (XXVII) and tetrahydropalmatine. 

A variety of aromatic diamines have been used for the synthesis of polyimides. It would be too time consuming to report all the pathways described in literature, so here only the most common ones are considered. The biggest part of these different methods leads to nitro compounds generally reduced using H2 or hydrazine monohydrate with catalytic amounts of Pd-C in refluxed ethanol or dioxane. The numbers in parentheses refer to Fig. 5.28 ... 

Carbohydrate Components of Antibiotics. Part III. Synthesis of 3.6-Dideoxy-3-dimethylamino- 3-D-glucose Hydrochloride Monohydrate the Absolute Configuration of Mycaminose, A. B. Foster, T. D. Inch, J. Lehmann, M. Stacey, and J. M. Webber, /. Chem. Soc., (1962) 2116-2118. 

The anhydrous salt is pyrophoric in air, or chars slowly in lower oxygen concentrations [1]. A safe and convenient synthesis of the dimeric monohydrate is described [2],... 

The synthesis of 4-trifhioromethylpyrimido[4,5-c]pyridazin-5,7-diones from 6-hydrazinouracils and l,l,l-trifluoropropane-2,3-dione monohydrates has been reported <06H1875>. Novel pyrimido[4,5-c]pyridazines have been synthesized and investigated as inhibitors of lymphocyte specific kinase <06BMCL4257 06H2037>. 

Kowalik, J. Sawka-Dobrowolska, W., and Glowiak, T., Synthesis, molecular structure, and absolute configuration of an optically active (l-amino-2-phe-nylethyl)phosphonic acid monohydrate, J. Chem. Soc., Chem. Commun., 446, 1984. 

Cyanoethylation of acrylonitrile with monohydric alcohols gives alkoxypropio-nitriles (Scheme 25). These nitriles can be converted into various types of carboxylic acids by hydrolysis, and they can be hydrogenated to give amines. Therefore, cyanoethylation of alcohols is an important reaction for the synthesis of drug intermediates and organic compounds of industrial interest. 

M. Krumpolc, B. G. DeBoer, and J. Rocek, A stable chromium(V) compound. Synthesis, properties and crystal structure of potassium bis(2-hydroxy-2-methylbutyrato)-oxochromate(V) monohydrate, J. Am. Chem. Soc., 100 (1978) 145-153. 

Polyethers and polyesters having methoxybenzalazine units with various alkylene groups (C4, C6 and Cg) in the main chain were synthesized from vanillin (7,8). The condensation reaction of 4,4 -alkylenedioxybis (3-methoxybenzaldehyde) [VI] with hydrazine monohydrate was applied to the synthesis of polyethers [VII] (Mn, 7.4 x 103 for C4, 7.3 x 103 for C6 and 4.1 x 103 for Cg derivatives), as shown in Scheme 3. Polyesters [IX] (77jnh, 0.35 dl/g for C4, 0.38 dl/g for C6 and 0.43 dl/g for Cg derivatives) were synthesized from 4,4 -dihydroxy-3,3 -dimethoxybenzalazine [VIII] and di-carboxylic acid chlorides by conventional low temperature solution polycondensation, as shown in Scheme 4. 

The addition of 1-lithiocyclopropyl phenyl sulfide to paraformaldehyde was the first step of an efficient synthesis of cyclobutanonc (8).169 The adduct 7 was rearranged with/Moluenesulfonic acid monohydrate in a mixture of tetralin and water while the liberated benzenethiol was trapped with mercury(II) chloride. 

Synthesis was by heating above 450 °C in evacuated quartz vessels of the stoichiometric components. The isostructural I MCl series underwent a phase transition in the range 350-410 °C, and became monohydrated in air. The K2MC15 series was also isostructural. 

Unfortunately the pyridine-catalyzed condensation is largely unsuccessful with unsaturated ketones. Furthermore, there are few examples of the use of monohydric penhols in this synthesis. 1-Naphthol affords the naphthopyran (81) with citral, though in poor yield, and 2-naphthol gives (82). The latter example is of interest since it provides a further illustration of the regiospecificity arising from resonance stabilization. 

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