Synthesis
The general procedure for the synthesis of tetrahydrothiopyran-4-one 1,1-dioxide from tetrahydrothiopyran-4-one was as follows: in Example 22, to a stirred solution of tetrahydrothiopyran-4-one (5.30 g, 43.1 mmol, Aldrich) in 50 mL of ethyl acetate, 32% peracetic acid (24 g, 110 mmol) was added dropwise at a slow rate, taking care to avoid refluxing. After completion of the dropwise addition, the reaction mixture was cooled to room temperature and the solid was collected by filtration to afford 1,1-dioxo-tetrahydro-thiopyran-4-one as a white solid (5.69 g, 89% yield).
References
[1] Journal of Organic Chemistry, 1995, vol. 60, # 6, p. 1665 - 1673
[2] Patent: US2007/129416, 2007, A1. Location in patent: Page/Page column 19/1
[3] Patent: EP2261213, 2010, A1. Location in patent: Page/Page column 60
[4] Journal of Organic Chemistry, 1998, vol. 63, # 24, p. 8952 - 8956
[5] European Journal of Medicinal Chemistry, 1999, vol. 34, # 2, p. 125 - 135
