Notes described above for 7a ( = 2, 4) except that the vols of H20 and DMF were increased 2.5-3 times.IV. S,S'-3,8-Diazaundecamethylenebis (dihydrogen phosphorothioate) (8a) was prepared by the procedure used for the prepn of 7a ( = 2,4).V. N,N'-(trans-l, 4-Cyclohexylene )bis(Y'-(czs-l,4-Cyclohexyienedimethylene)bis(S-2-aminoethyl lithium hydrogen phosphorothioate) (13a) was prepd in the manner described for 12a (re = 1). 2,2'-[
A series of alpha-quinoxalinyl-N-substitute nitrone 1,4-dioxides has been synthesize and evaluated as antibacterial and antiprotozoal agents. Structure-activity relationships are discussed. Of the compounds tested, alpha-(3-methyl-2-quinoxalinyl)-N-methylnitrone 1,4-dioxide (2) was the most active agent in vivo against the gram-negative and the gram-positive organisms.
3.2-3.4» 0 Taken with a Varían A-60 spectrometer. 1 External TMS as standard. c Internal TMS as standard. d Overlapped by CgHs signals.' Jph = 3 Hz. / Complex multiplet. " Overlapped by phenethyl CHs signals.as well.8 The nature of the P substituents may also play a role in preventing dimerization of phospholium ions; thus, the , -dimethyl derivative of the 3methylphospholium ion appears to be dimeric7 while the , -dibenzyl derivative (2) remains monomeric.It would seem to be necessary to consider carefully the structure assigned to a new phosphole salt in view of these results.The two 31P signals of the dimers are due to the presence of 3-phospholenium and 2-phospholenium moieties. In the dimers examined, the signals are separated by only 1-1.5 ppm. Normally, isomeric 3-phospholenium and 2-phospholenium ions have a greater spread in their 31P shifts (e.g., for the 1,1,3trimethyl ions, -47.1 and -54.5 ppm, respectively).
Ethyl acetoacetate reacted with 3‐bromo‐1,1,1‐trifluoro‐2‐propanone in the presence of base to give 3 ‐carbethoxy‐4,5‐dihydro‐4‐hydroxy‐2‐methyl‐4‐trifluoromethylfuran (I). Acid catalyzed dehydration of I gave the corresponding furan (III). Saponification of III gave 2‐methyl‐4‐trifluoromethyl‐3‐furoic acid which was decarboxylated to yield 2‐methyl‐4‐trifluoromethylfuran (V) for which a structure proof is presented. Conversion of the methyl groups of III and V to formyl groups is described.
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