Thin films of (BEDT-TTF)2Cu(NCS)2 are prepared by the electrochemical oxidation of BEDT-TTF at a large current density. The films are composed of numerous platelets, which are set on edge and loosely packed on the anodes. The X-ray diffraction suggests that the product contains both amorphous regions and κ-type and other crystals. The ESR and conductivity are discussed in terms of the presence of amorphous regions.
The preparation of 1-trifluoromethylphenothiazine is reported. Methanolic basic hydrolysis of 1and 3-trifluoromethylphenothiazines to the corresponding ortho esters of phenothiazinecarboxylic acids is described. 2-, 3and 4-Trifluoromethylphenothiazines have re-SCHEME 1 ceived considerable attention in past years due mainly to the interest in their antioxidant properties and to the psychotropic action of their derivatives (2-9). As part of a continuing program to develop new pharmacological Hs)5J 111 agents, we required the hitherto unreported l-trifluoromethyl isomer. We now wish to report the synthesis of I II her NO2 HZN NnOll 1-trifluoromethylphenothiazine by the Smiles rearrangement (10) and the preparation of a new class of compounds, ortho esters of phenothiazinecarboxylic acids, by fluoromethylphenothiazines in methanol. Our approach to 1-trifluoromethylphenothiazine (VIII, Scheme 1) commenced with the preparation of 2-bromogood yield from 2-bromo-3-nitrobenzoic acid (I) and sulfur the basic hydrolysis [CF3 + C(OCH3),] of 1-and 3-tri-@fS% / \ ; ; ; ) I CHO V l 11(:1 JAs expected, acid hydrolysis of l-trifluoromethylphenothiazine (VIII) provided the known carboxylic acid (IX, Scheme 2). Unexpectedly, however, the reaction of VIII and methanolic potassium hydroxide produced an additional product, trimethyl orthophenothiazine-l-carboxylate (X), in 47% yield. There appears to be no previous
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