68965-44-6

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Methyl 2-(t-butoxycarbonylmethylene)-1,3-dithietane-4-carboxylate (1.05 g) is reacted with difluoromethylsulphenyl chloride, which was synthesized from difluoromethyl benzyl thioether (1.74 g) and chlorine, in dichloromethane (5 ml) at room temperature in the presence of pyridine (0.65 ml) until no starting carboxylate is detected in the reaction mixture. The mixture is then washed with a 5% sodium thiosulfate solution and 10% HCl, dried, and concentrated in vacuo to give methyl 2-(1-t-butoxycarbonyl-1-difluoromethylthiomethylene)-1,3-dithietane-4-carboxylate. The mixture is then washed with a 5% sodium thiosulfate solution and 10% HCl dried concentrated in vacuo

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: One equivalent of 40% by weight of sodium hydroxide in water was mixed with one equivalent of benzyl mercaptan with R-22 (1.1 molar equivalents) at 60° C. for 1 h. The tests are carried out in a 500 ml Hastelloy reactor at an autogenous pressure at 60° C. The pressure is 3.5 bar. A chemical yield of 75%, by quantitative determination by 19F NMR, is obtained over two tests carried out under the same conditions. The tests are carried out in a 500 ml Hastelloy reactor at an autogenous pressure at 60° C A chemical yield of 75%, by quantitative determination by 19F NMR, is obtained over two tests

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Methyl 2-(t-butoxycarbonylmethylene)-1,3-dithietane-4-carboxylate (1.05 g) is reacted with difluoromethylsulphenyl chloride, which was synthesized from difluoromethyl benzyl thioether (1.74 g) and chlorine, in dichloromethane (5 ml) at room temperature in the presence of pyridine (0.65 ml) until no starting carboxylate is detected in the reaction mixture. The mixture is then washed with a 5% sodium thiosulfate solution and 10% HCl, dried, and concentrated in vacuo to give methyl 2-(1-t-butoxycarbonyl-1-difluoromethylthiomethylene)-1,3-dithietane-4-carboxylate. The mixture is then washed with a 5% sodium thiosulfate solution and 10% HCl dried concentrated in vacuo

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Methyl 2-(t-butoxycarbonylmethylene)-1,3-dithietane-4-carboxylate (1.05 g) is reacted with difluoromethylsulphenyl chloride, which was synthesized from difluoromethyl benzyl thioether (1.74 g) and chlorine, in dichloromethane (5 ml) at room temperature in the presence of pyridine (0.65 ml) until no starting carboxylate is detected in the reaction mixture. The mixture is then washed with a 5% sodium thiosulfate solution and 10% HCl, dried, and concentrated in vacuo to give methyl 2-(1-t-butoxycarbonyl-1-difluoromethylthiomethylene)-1,3-dithietane-4-carboxylate. The mixture is then washed with a 5% sodium thiosulfate solution and 10% HCl dried concentrated in vacuo

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: One equivalent of 40% by weight of sodium hydroxide in water was mixed with one equivalent of benzyl mercaptan with R-22 (1.1 molar equivalents) at 60° C. for 1 h. The tests are carried out in a 500 ml Hastelloy reactor at an autogenous pressure at 60° C. The pressure is 3.5 bar. A chemical yield of 75%, by quantitative determination by 19F NMR, is obtained over two tests carried out under the same conditions. The tests are carried out in a 500 ml Hastelloy reactor at an autogenous pressure at 60° C A chemical yield of 75%, by quantitative determination by 19F NMR, is obtained over two tests

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Methyl 2-(t-butoxycarbonylmethylene)-1,3-dithietane-4-carboxylate (1.05 g) is reacted with difluoromethylsulphenyl chloride, which was synthesized from difluoromethyl benzyl thioether (1.74 g) and chlorine, in dichloromethane (5 ml) at room temperature in the presence of pyridine (0.65 ml) until no starting carboxylate is detected in the reaction mixture. The mixture is then washed with a 5% sodium thiosulfate solution and 10% HCl, dried, and concentrated in vacuo to give methyl 2-(1-t-butoxycarbonyl-1-difluoromethylthiomethylene)-1,3-dithietane-4-carboxylate. The mixture is then washed with a 5% sodium thiosulfate solution and 10% HCl dried concentrated in vacuo