S-0 stretches in SOF2 and S0C12 occur at 1312 and 1229 cm-1, respectively.22 Kagarise23 was able to demonstrate a linear relationship between carbonyl stretching frequency and the sum of the electronegativity values (Gordy scale24) of atoms X and Y in molecules of the type XCOY. However, when this was applied to structurally similar sulfinyl compounds,25 the points fell on a smooth curve and it was noted that changes in electronegativities of substituents in XSOY had smaller effects on S-O stretching frequency than on C-0 analogs. This is in agreement with Moffitt26 who showed that there is a relatively small variation in bond order in many XSOY compounds. When the elec-tronegativities22,23 of the trifluoromethylsulfinyl halides are superimposed on this curve, the absorption bands at 1268, 1238, and 1235 cm-1 for CF3S(0)F, CF3S(0)C1, and CF3S(0)Br, respectively, correspond to the S-0 stretching frequency. By the same process, bands at 1260 and 1258 cm-1 in the spectra of C2F5S(0)F and z-C3F7S(0)F are attributable to S-0 stretch. Based (22) D.
Fluoroperoxysulfuryl fluoride, FS0200F, was the first compound reported to contain the fluoroperoxy, OOF, group. This compound was prepared1 by the photolytic reaction of sulfur trioxide, S03, and oxygen difluoride, OF2, and by the reaction of sulfur dioxide, S02, and dioxygen difluoride.2 Thompson3 reported that the direct fluorination of salts of trifluoroacetic acid, CFsC02H, produced a number of products including very small amount of fluoroperoxytrifluoromethane, CF3OOF, and fluoroperoxypentafluoroethane, CFS-CF2OOF. 1-and 2-fluoroperoxyperfluoropropanes have also been reported4 5to result from the reaction of perfluoropropene, CsFe, and 02F2. At the time this research was initiated a convenient method for the preparation of a fluoroperoxyperfluoroalkane was not available.Anderson and Fox6 reported that oxygen difluoride, OF2, and carbonyl fluoride, COF2, react in the presence of cesium fluoride, CsF, catalyst to give good yields of bis(trifluoromethyl) trioxide, CF3OOOCF3, and have suggested that the formation of CF3OOOCF3 proceeds by the mechanism COF2 + CsF -> Cs+OCF3-They, however, did not detect CF3OOF in their experiments.We have additional proof of the validity of this mech-
Proton chemical shifts are reported for 14 products and intermediates involved in the formation of 1,3,5,7-tetranitro-l,3,5,7-tetraazacyclooctane (HMX) from the nitrolysis of hexamethylenetetramine (hexamine). These include three hexamine derivatives and six cyclic and five linear nitramines. Geminal proton spin coupling is observed in three cases.In the present work, we obtained proton magnetic resonance (pmr) spectral data on several compounds which have been characterized as products or intermediates in the formation of 1,3,5,7-tetranitro-1,3,5,7-tetraazacyclooctane (HMX) from the nitrolysis of hexamethylenetetramine (hexamine). This reaction was discussed by Urbanski ( 3 ) and Wright ( 4 ) , among others.' To whom correspondence should be addressed.
The typical phencyclidine sample found in clandestine laboratories can be contaminated by the presence of unreacted precursors and large amounts of impurities and by-products. Although this may involve an extensive “cleanup” procedure before phencyclidine identification, the additional analysis of the sample for the impurities will often confirm the synthetic process employed. A gas chromatography/mass spectrometry procedure has been developed in which the 13 major components, including phencyclidine and piperidinocyclohexane carbonitrile, found in these typical clandestine mixtures, may be screened for and identified. The data obtained from this analysis are consistently used as an aid to the successful prosecution of “intent to manufacture” cases.
A submission to the Drug Enforcement Administration North Central Laboratory of a substance believed to be a structural analog of methaqualone hydrochloride precipitated an interest in being able to obtain a rapid and positive identification of such compounds. Both mass spectrometry and proton NMR spectroscopy (1-dimensional) provided evidence to suggest that the structural analog possessed a second methyl group in the molecule, relative to methaqualone, and that the methyl group was attached to the existing methylsubstituted phenyl ring. By application of proton 2-dimensional (2-D) NMR techniques, specifically the homonuclear shift correlation spectroscopy (COSY) and 2-D NOE (NOESY), the precise location of the methyl group in this unknown methaqualone analog was established and shown to have the structure 2.
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