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Methoxycarbonylmethyldisulfanyl-acetic acid methyl ester synthesis

4synthesis methods
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Yield:1665-64-1 99%

Reaction Conditions:

with TiO2/MoS2 (10:1 molar ratio of Ti to Mo) nanocomposite;air in ethanol at 20; for 8 h;Irradiation;Green chemistry;

Steps:

General procedure for the synthesis of disulfides

General procedure: TiO2/MoS2 (10:1 molar ratio, 10 mg) was added to a solution of thiol 1 (1 mmol) in ethanol (1 mL). The reaction mixture was stirred under a 14W CFL irradiation at a distance of 10 cm at room temperature for a certain time. After reaction (monitored by thin-layer chromatography, TLC), ethyl acetate was added, and the solid catalyst was recovered by centrifugation. The reaction mixture was extracted with ethyl acetate and washed with water. The combined organic phase was then dried over Na2SO4 and concentrated under reduced pressure to give the crude residue, which was purified by column chromatography with petroleum ether-ethyl acetate to afford the pure product 2. The recovered catalyst was then washed with ethanol and deionized water, dried under vacuum, and reused for the next run.

References:

Liu, Wenjie;Wang, Cancan;Huang, Yibo;Chen, Qun;Wang, Liang;He, Mingyang [Synthetic Communications,2016,vol. 46,# 15,p. 1268 - 1274] Location in patent:supporting information