A Convenient Multigram Synthesis of DABSO Using Sodium Sulfite as SO2 Source
Author(s) -
Seger Van Mileghem,
Wim M. De Borggraeve
Publication year - 2017
Publication title -
organic process research and development
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.904
H-Index - 109
eISSN - 1520-586X
pISSN - 1083-6160
DOI - 10.1021/acs.oprd.7b00083
Subject(s) - anhydrous , sodium sulfite , chemistry , sulfite , sulfur dioxide , stoichiometry , yield (engineering) , sulfur , sodium , dabco , inorganic chemistry , organic chemistry , catalysis , materials science , metallurgy
A convenient synthesis of DABCO·(SO2)2 (abbreviated as DABSO) is reported. Using a two-chamber set-up, sulfur dioxide is generated in one chamber and consumed in the other. This closed system overcomes safety issues related to working with toxic SO2 gas. Pressure build-up is avoided by gradually generating the gas using sodium sulfite as precursor. Moreover, only near-stoichiometric amounts of SO2 are required for this protocol. The use of anhydrous solvents is not necessary and every step is performed at room temperature. A scale-up was carried out on a 10 gram scale which, after overnight drying, resulted in a quantitative yield.status: publishe
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