[CH3:1][C:2]([CH3:8])=[CH:3][C:4]([O:6][CH3:7])=[O:5].N1CCCCC1.[SH:15][CH2:16][CH2:17][C:18]([O:20][CH3:21])=[O:19].CCOCC>CO>[CH3:7][O:6][C:4](=[O:5])[CH2:3][C:2]([S:15][CH2:16][CH2:17][C:18]([O:20][CH3:21])=[O:19])([CH3:8])[CH3:1]To a well-stirred mixture of methyl 3-methylbut-2-enoate (50.0 g, 438 mmol), 40% Triton B in MeOH (5 mL) and piperidine (4 mL) were added dropwise at 0° C., then methyl 3-mercaptopropanoate (50 g, 396 mmol) was added. After stirring for 24 h at 60° C., Et2O (500 mL) was added, and the organic phase washed thoroughly with 10% H2SO4 (150 mL), sat. NaHCO3 (150 mL), and brine (200 mL) successively, dried over Na2SO4 and evaporated under vacuum to give the title compound as a colorless oil (90.1 g, 97.23%).
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