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The general procedure for the hydrothiocarboxylation of acetylenes with thiols and carbon monoxide is as follows: In a 50 mL stainless steel autoclave with a magnetic stirring bar under argon atmosphere were placed Pt(PPh3)4 (3 mol%), acetonitrile (5 mL), acetylene (5 mmol), and cyclohexanethiol (5 mmol). Carbon monoxide was purged three times and then changed at 30 atm. The reaction was conducted with magnetic stirring for 2 h upon heating at 120 °C. After the carbon monoxide was purged, the resulting mixture was filtered through Celite and concentrated in vacuo. Purification of the product was carried out by MPLC (silica gel, 25-40 µm, length 310 mm, i.d. 25 mm, eluent hexane:Et2O) 4:1
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The general procedure for the hydrothiocarboxylation of acetylenes with thiols and carbon monoxide is as follows: In a 50 mL stainless steel autoclave with a magnetic stirring bar under argon atmosphere were placed Pt(PPh3)4 (3 mol%), acetonitrile (5 mL), acetylene (5 mmol), and cyclohexanethiol (5 mmol). Carbon monoxide was purged three times and then changed at 30 atm. The reaction was conducted with magnetic stirring for 2 h upon heating at 120 °C. After the carbon monoxide was purged, the resulting mixture was filtered through Celite and concentrated in vacuo. Purification of the product was carried out by MPLC (silica gel, 25-40 µm, length 310 mm, i.d. 25 mm, eluent hexane:Et2O) 4:1).
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