Abstract:Was endlich d betrifft, so fiihrt dessen Spaltung in lihnlicher Weise zu einem Destillat, aus dem beim Rektifizieren Schwefelkohlenstoff, dann in sehr kleinerMenge das D i t h i o -c a r b a m i n a t C,H,,,N.CSSH, NHC,H,, (Schmp. 170~) und als Hauptfraktion der unter 13 mm bei 210--212~ siedende T h i o h a r n s t o f f C,H,,N.CS.NC,H,, vom Schmp. 58O, der auf diesem Wege auch sehr bequem darstellbar ist, herausgeholt werden konnte. Und als nun auf Grund dieser Erfahrungen das oben bei der Nitrophenyl-schwef… Show more
“…Reduction of l a with sodium sulfite gave the sodium sulfinate (7); the sulfinic acid 8 was obtained by acidification and continuous extraction of a solution of 7 , and was readily converted back to l a by brief chlorination. Reaction of the sodium sulfinate 7 with ethyl iodide gave a modest yield of ethyl 2-hydroxyethyl sulfone (9), identical to a sample prepared from sodium ethanesulfinate and ethylene chlorohydrin (25). These observations clearly establish the structure l a beyond reasonable doubt.…”
“…Reduction of l a with sodium sulfite gave the sodium sulfinate (7); the sulfinic acid 8 was obtained by acidification and continuous extraction of a solution of 7 , and was readily converted back to l a by brief chlorination. Reaction of the sodium sulfinate 7 with ethyl iodide gave a modest yield of ethyl 2-hydroxyethyl sulfone (9), identical to a sample prepared from sodium ethanesulfinate and ethylene chlorohydrin (25). These observations clearly establish the structure l a beyond reasonable doubt.…”
“…The literature records a melting point of 93-94°. 20 Reaction of 4-t-butyl-2-methoxymethyl-6-methylbromobenzene with n-butyllithium. To a dry flask containing 100 ml.…”
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