Methyl methacrylate, a cyclic olefin, and two alk-1-enes are efficiently converted into their corresponding epoxides by nt-chloroperbenzoic acid a t elevated temperatures in the presence of a small amount of a radical inhibitor, which prevents thermal decomposition of the peracid.:@-H20Hwas considered ; however, thermal decomposition of the peracid becomes a problem and the possibility that it might be suppressed in the presence of some radical inhibitor was investigated.?IN the course of an investigation directed towards a total synthesis of tetrodotoxin,l conversion of the olefin (I) into the epoxide (11) was required. This seemingly easy step turned out to be difficult because the double bond in the L b Ht) iiF ' olefin (I) has exceptionally poor reactivity towards peracids AC ( 1 ) such as m-chloroperbenzoic acid, peracetic acid, and performic acid. Epoxidation a t an elevated temperature Ac (II) t T. M. Luong and D. Lefort observed that the decomposition of perbenzoic acid in cyclohexane at 80 "C is suppressed in the presence However, these inhibitors are not efiective enough for the of 9-benzoquinone or hydroquinone (Bull. Soc. chim. France, 1962, 827). present purpose.$ We are indebted to Sumitomo Chemical Co., Ltd., for gifts of the radical inhibitors.3 Epoxidation of (I) with m-chloroperbenzoic acid (excess) a t 90 "C in the absence of the radical inhibitor gave a complex mixture.
Fullerene-poly(ethylene dioxythiophene) (polyEDOT) composite films consisting of 3,4-ethyeledioxythiophene (EDOT) and a thiophene derivative of C 60 fullerene (ThC 60 ) or C 60 fullerene were fabricated on a transparent indium-tin-oxide (ITO) electrode by electrochemical polymerization of the electrolyte solution of ThC 60 (or C 60 ) and EDOT. Incorporation of the C 60 fullerene moiety in the polythiophene film was strongly suggested from absorption spectra of the composite film. We have found a higher degree of incorporation of the C 60 fullerene moiety into the ThC 60 -polyEDOT film, as compared with the C 60 -polyEDOT film. In the presence of methylviologen as an electron acceptor, the as-prepared C 60 -polyEDOT and ThC 60 -polyEDOT composite films generated stable cathodic photocurrents in the 400 -700 nm region with broad peaks. The photocurrent intensity and the internal photon-to-current quantum efficiency of the ThC 60 -polyEDOT composite film were considerably larger than those of C 60 -polyEDOT and polyEDOT films. The thiophene unit of ThC 60 was confirmed to be quite effective for a stable incorporation of the C 60 fullerene moiety in the film and a higher photocurrent generation.
A new deposition technique for molybdenum silicide films is presented whereby the films are deposited by magnetron‐d‐c‐reactive sputtering using a Mo target in a silane argon atmosphere. The influence of sputtering conditions upon the film properties was investigated by utilizing mass spectroscopy, Auger electron spectroscopy, and x‐ray diffractometry. Films with various Si/Mo atomic ratios up to 1.9 were obtained by controlling the sputtering power and the silane partial pressure. The crystal structures were found to be continuously transformed from Mo‐rich silicides to Si‐rich ones, including
Mo3normalSi
,
Mo5Si3
, and
MoSi2
, with increasing Si/Mo atomic ratio.
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