Synthesis
Ethyl S-2-(dimethylamino)butyryl thiolate was dissolved in THF 3L. Under nitrogen protection, methyl iodide was added dropwise, and the process was maintained at an internal temperature of 20-30 °C. After the completion of the dropwise addition, the reaction was allowed to stand overnight at room temperature. TLC showed the reaction was complete. Filtered, washed with THF, and dried under reduced pressure at 30 ° C to give a white solidS-iodinated butyrylthiocholine.
Purification Methods
Recrystallise S-butyryl thiocholine iodide from propan-1-ol and dry it in vacuo; store it in the dark under N2. The bromide has m 150o (from Me2CO) or m 140-143o (from butan-1-ol). [Gillis Chem Ind (London) 111 1957, Hansen Acta Chem Scand 11 537 1957, Beilstein 4 IV 1586.]
References
[1] Patent: CN108586300, 2018, A. Location in patent: Paragraph 0039; 0040; 0041
[2] Acta Chemica Scandinavica (1947-1973), 1957, vol. 11, p. 537,538
[3] Chemistry and Industry (London, United Kingdom), 1957, p. 111
[4] Acta Chemica Scandinavica (1947-1973), 1957, vol. 11, p. 537,538
[5] Chemistry and Industry (London, United Kingdom), 1957, p. 111
