1,2-二氯氟乙烷

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A mixture of 217.8 g of the 2-mercaptophenylsulfonamide triethylamine salt obtained in accordance with Example H6 and 101 g of 1,2-dichloro-1-fluoroethane in 950 ml of methanol is stirred for 24 hours at a temperature of +65° C. to +70° C. and is then stirred in an autoclave for a further 24 hours at +95° C. to +100° C. The reaction mixture is then evaporated and the residue is triturated with water. Extracting the mixture with ethyl acetate, washing the extract with water, drying it over sodium sulfate and evaporating it and purifying the residue by chromatography with methylene chloride gives 99.5 g (49.2% of theory) of 2-(2-chloro-2-fluoroethylthio)-phenylsulfonamide having a melting point of +88° C. to +89° C. is then stirred in an autoclave for a further 24 hours at +95° C. to +100° C The reaction mixture is then evaporated the residue is triturated with water Extracting the mixture with ethyl acetate washing the extract with water drying it over sodium sulfate evaporating it purifying the residue by chromatography with methylene chloride

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A mixture of 217.8 g of the triethylamine salt of 2-mercaptophenylsulfonamide obtained in accordance with Example P6 and 101 g of 1,2-dichloro-1-fluoroethane in 950 ml of methanol is stirred in an autoclave for 24 hours at a temperature of from +65° C. to +70° C. and for a further 24 hours at from +95° C. to +100° C. The reaction mixture is then concentrated by evaporation and the residue is stirred with water. By extracting with ethyl acetate, washing with water, drying over sodium sulfate, concentrating by evaporation and purifying the residue by chromatography with methylene chloride, 99.5 g (49.2% of the theoretical yield) of 2-(2-chloro-2-fluoroethylthio)-phenylsulfonamide having a melting point of from +88° C. to +89° C. are obtained. The reaction mixture is then concentrated by evaporation the residue is stirred with water By extracting with ethyl acetate washing with water drying over sodium sulfate concentrating by evaporation purifying the residue by chromatography with methylene chloride, 99.5 g (49.2% of the

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A mixture of 217.8 g of the 2-mercaptophenylsulfonamide triethylamine salt obtained in accordance with Example H6 and 101 g of 1,2-dichloro-1-fluoroethane in 950 ml of methanol is stirred for 24 hours at a temperature of +65° C. to +70° C. and is then stirred in an autoclave for a further 24 hours at +95° C. to +100° C. The reaction mixture is then evaporated and the residue is triturated with water. Extracting the mixture with ethyl acetate, washing the extract with water, drying it over sodium sulfate and evaporating it and purifying the residue by chromatography with methylene chloride gives 99.5 g (49.2% of theory) of 2-(2-chloro-2-fluoroethylthio)-phenylsulfonamide having a melting point of +88° C. to +89° C. is then stirred in an autoclave for a further 24 hours at +95° C. to +100° C The reaction mixture is then evaporated the residue is triturated with water Extracting the mixture with ethyl acetate washing the extract with water drying it over sodium sulfate evaporating it purifying the residue by chromatography with methylene chloride

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A mixture of 217.8 g of the triethylamine salt of 2-mercaptophenylsulfonamide obtained in accordance with Example P6 and 101 g of 1,2-dichloro-1-fluoroethane in 950 ml of methanol is stirred in an autoclave for 24 hours at a temperature of from +65° C. to +70° C. and for a further 24 hours at from +95° C. to +100° C. The reaction mixture is then concentrated by evaporation and the residue is stirred with water. By extracting with ethyl acetate, washing with water, drying over sodium sulfate, concentrating by evaporation and purifying the residue by chromatography with methylene chloride, 99.5 g (49.2% of the theoretical yield) of 2-(2-chloro-2-fluoroethylthio)-phenylsulfonamide having a melting point of from +88° C. to +89° C. are obtained. The reaction mixture is then concentrated by evaporation the residue is stirred with water By extracting with ethyl acetate washing with water drying over sodium sulfate concentrating by evaporation purifying the residue by chromatography with methylene chloride, 99.5 g (49.2% of the

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A mixture of 217.8 g of the triethylamine salt of 2-mercaptophenylsulfonamide obtained in accordance with Example P6 and 101 g of 1,2-dichloro-1-fluoroethane in 950 ml of methanol is stirred in an autoclave for 24 hours at a temperature of from +65° C. to +70° C. and for a further 24 hours at from +95° C. to +100° C. The reaction mixture is then concentrated by evaporation and the residue is stirred with water. By extracting with ethyl acetate, washing with water, drying over sodium sulfate, concentrating by evaporation and purifying the residue by chromatography with methylene chloride, 99.5 g (49.2% of the theoretical yield) of 2-(2-chloro-2-fluoroethylthio)-phenylsulfonamide having a melting point of from +88° C. to +89° C. are obtained. The reaction mixture is then concentrated by evaporation the residue is stirred with water By extracting with ethyl acetate washing with water drying over sodium sulfate concentrating by evaporation purifying the residue by chromatography with methylene chloride, 99.5 g (49.2% of the

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A mixture of 217.8 g of the triethylamine salt of 2-mercaptophenylsulfonamide obtained in accordance with Example P6 and 101 g of 1,2-dichloro-1-fluoroethane in 950 ml of methanol is stirred in an autoclave for 24 hours at a temperature of from +65° C. to +70° C. and for a further 24 hours at from +95° C. to +100° C. The reaction mixture is then concentrated by evaporation and the residue is stirred with water. By extracting with ethyl acetate, washing with water, drying over sodium sulfate, concentrating by evaporation and purifying the residue by chromatography with methylene chloride, 99.5 g (49.2% of the theoretical yield) of 2-(2-chloro-2-fluoroethylthio)-phenylsulfonamide having a melting point of from +88° C. to +89° C. are obtained. The reaction mixture is then concentrated by evaporation the residue is stirred with water By extracting with ethyl acetate washing with water drying over sodium sulfate concentrating by evaporation purifying the residue by chromatography with methylene chloride, 99.5 g (49.2% of the

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A mixture of 217.8 g of the 2-mercaptophenylsulfonamide triethylamine salt obtained in accordance with Example H6 and 101 g of 1,2-dichloro-1-fluoroethane in 950 ml of methanol is stirred for 24 hours at a temperature of +65° C. to +70° C. and is then stirred in an autoclave for a further 24 hours at +95° C. to +100° C. The reaction mixture is then evaporated and the residue is triturated with water. Extracting the mixture with ethyl acetate, washing the extract with water, drying it over sodium sulfate and evaporating it and purifying the residue by chromatography with methylene chloride gives 99.5 g (49.2% of theory) of 2-(2-chloro-2-fluoroethylthio)-phenylsulfonamide having a melting point of +88° C. to +89° C. is then stirred in an autoclave for a further 24 hours at +95° C. to +100° C The reaction mixture is then evaporated the residue is triturated with water Extracting the mixture with ethyl acetate washing the extract with water drying it over sodium sulfate evaporating it purifying the residue by chromatography with methylene chloride

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A mixture of 217.8 g of the triethylamine salt of 2-mercaptophenylsulfonamide obtained in accordance with Example P6 and 101 g of 1,2-dichloro-1-fluoroethane in 950 ml of methanol is stirred in an autoclave for 24 hours at a temperature of from +65° C. to +70° C. and for a further 24 hours at from +95° C. to +100° C. The reaction mixture is then concentrated by evaporation and the residue is stirred with water. By extracting with ethyl acetate, washing with water, drying over sodium sulfate, concentrating by evaporation and purifying the residue by chromatography with methylene chloride, 99.5 g (49.2% of the theoretical yield) of 2-(2-chloro-2-fluoroethylthio)-phenylsulfonamide having a melting point of from +88° C. to +89° C. are obtained. The reaction mixture is then concentrated by evaporation the residue is stirred with water By extracting with ethyl acetate washing with water drying over sodium sulfate concentrating by evaporation purifying the residue by chromatography with methylene chloride, 99.5 g (49.2% of the