Ramanspektroskopische Untersuchungen an Derivaten der Sulfoxylsäure und der Thioschwefligen Säure

Abstract

Es werden die Raman‐Spektren von Estern und von Säureamiden der Sulfoxylsäure und der Thioschwefligen Säure mitgeteilt. Mit den beobachteten Spektren sind für die Sulfoxylsäure‐Derivate die Formeln RO·S·OR bzw. R2N·S·NR2 gut zu vereinbaren. Für die Abkömmlinge der Thioschwefligen Säure sind die symmetrischen Formeln RO·S·S·OR bzw. R2N·S·S·NR2 am wahrscheinlichsten.

Gas phase structure and vibrational spectra of dimethoxysulfane (CH3O)2S

“…A second distillation at normal pressure resulted in pure dimethyl sulfoxylate in 34% yield (4.9 g) as a colorless liquid, the vapor of which is strongly lachrymatory (bp 74"C/1013 mbar; mp -67°C). Analysis: C (calcd) 25.52%, (found) 25.61%, H (calcd) 6.42%, (found) 6.50%; 'H NMR spectrum: s 3.96 ppm (CDCl,; 80 MHz). Dimethyld6 sulfoxylate was prepared following the above procedure; 12.5 g of di[imidazolyl-I-]sulfide reacted with 6.1 mL of methanold (Fluka, >99.5 atom-% D) to yield 2.4 g of pure dimethyl-d, sulfoxylate (32%) (bp 73"C/1013 mbar).…”

“…712 cm-I [25] C2HsOSOC,H,: The structural fragment OSO of (CH30),S may be compared to the SF2 molecule, the stretching vibrations of which occur at 813 and 839 cm-' in the vapor phase [28]. The small difference of only 3% causes us to expect v, (SO) and v,, (SO) of (CH30),S to be closely neighboring in the spectra.…”

Synthesis of New Cyclic Thionosulfites

“…It was not until 1964 that Thompson and co-workers 2,3 were able to confirm that this functionality could potentially exist in two separate constitutional forms, namely dialkoxy disulfides 1 and a branch-bonded arrangement as thionosulfites 2. Other isomers such as the thiosulfonate ester (RSO 2 SR) previously proposed by Zinner 4 were readily ruled out by their 1 HNMR spectra, while other work [5][6][7][8] failed to fully distinguish 1 from 2.…”