1-苄基硫烷基-2-(氯甲基)苯

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

实验步骤: To a suspension of 9.9 g of potassium t-butoxide in 100 ml of DMF under a N2 atmosphere was added portion wise 6 g of 1,2,4-triazole. After stirring at ambient temperature for one hour, a solution of 20 g of 2-benzylmercaptobenzyl chloride in 15 ml of DMF was added dropwise and the suspension was heated at 70° C. for 4 hours, then stirred at 25° C. 16 hours. After pouring the suspension into excess ice-water the residue was extracted with methylene chloride, dried (MgSO4), and the solvent was evaporated in vacuo to an oil residue which solidified to 14.5 g of the subject compound when triturated with 1-chlorobutane; m.p. 65°-68° C. the suspension was heated at 70° C. for 4 hours stirred at 25° C 16 hours was extracted with methylene chloride dried (MgSO4) the solvent was evaporated in vacuo to an oil residue which triturated with 1-chlorobutane

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

实验步骤: To a suspension of 9.9 g of potassium t-butoxide in 100 ml of DMF under a N2 atmosphere was added portion wise 6 g of 1,2,4-triazole. After stirring at ambient temperature for one hour, a solution of 20 g of 2-benzylmercaptobenzyl chloride in 15 ml of DMF was added dropwise and the suspension was heated at 70° C. for 4 hours, then stirred at 25° C. 16 hours. After pouring the suspension into excess ice-water the residue was extracted with methylene chloride, dried (MgSO4), and the solvent was evaporated in vacuo to an oil residue which solidified to 14.5 g of the subject compound when triturated with 1-chlorobutane; m.p. 65°-68° C. the suspension was heated at 70° C. for 4 hours stirred at 25° C 16 hours was extracted with methylene chloride dried (MgSO4) the solvent was evaporated in vacuo to an oil residue which triturated with 1-chlorobutane

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

实验步骤: To a solution of 1.35 g of potassium-tertbutoxide in 25 mL of dimethylformamide, cooled to 0° C., was added 0.92 mL of 2-pyrrolidinone. As a white precipitate formed, the mixture was stirred for 10 minutes, and 3.0 g of 2-phenylmethylthio chloromethyl benzene was added in one portion. The resulting solution was allowed to warm to room temperature, stirred for 1 hour, poured into water, and extracted with methylene chloride. The organic layer was washed well with water, dried over magnesium sulfate, filtered, and the filtrate evaporated to leave 3.0 g of a yellow oil. As a white precipitate formed stirred for 1 hour extracted with methylene chloride The organic layer was washed well with water dried over magnesium sulfate filtered the filtrate evaporated

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

实验步骤: To a solution of 1.35 g of potassium-tertbutoxide in 25 mL of dimethylformamide, cooled to 0° C., was added 0.92 mL of 2-pyrrolidinone. As a white precipitate formed, the mixture was stirred for 10 minutes, and 3.0 g of 2-phenylmethylthio chloromethyl benzene was added in one portion. The resulting solution was allowed to warm to room temperature, stirred for 1 hour, poured into water, and extracted with methylene chloride. The organic layer was washed well with water, dried over magnesium sulfate, filtered, and the filtrate evaporated to leave 3.0 g of a yellow oil. As a white precipitate formed stirred for 1 hour extracted with methylene chloride The organic layer was washed well with water dried over magnesium sulfate filtered the filtrate evaporated

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

实验步骤: To a solution of 1.35 g of potassium-tert-butoxide in 25 mL of dimethylformamide, cooled to 0° C., was added 0.92 mL of 2-pyrrolidinone. As a white precipitate formed, the mixture was stirred for 10 minutes, and 3.0 g of 2-phenylmethylthio chloromethyl benzene was added in one portion. The resulting solution was allowed to warm to room temperature, stirred for 1 hour, poured into water, and extracted with methylene chloride. The organic layer was washed well with water, dried over magnesium sulfate, filtered, and the filtrate evaporated to leave 3.0 g of a yellow oil. As a white precipitate formed stirred for 1 hour extracted with methylene chloride The organic layer was washed well with water dried over magnesium sulfate filtered the filtrate evaporated

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

实验步骤: To a suspension of 9.9 g of potassium t-butoxide in 100 ml of DMF under a N2 atmosphere was added portion wise 6 g of 1,2,4-triazole. After stirring at ambient temperature for one hour, a solution of 20 g of 2-benzylmercaptobenzyl chloride in 15 ml of DMF was added dropwise and the suspension was heated at 70° C. for 4 hours, then stirred at 25° C. 16 hours. After pouring the suspension into excess ice-water the residue was extracted with methylene chloride, dried (MgSO4), and the solvent was evaporated in vacuo to an oil residue which solidified to 14.5 g of the subject compound when triturated with 1-chlorobutane; m.p. 65°-68° C. the suspension was heated at 70° C. for 4 hours stirred at 25° C 16 hours was extracted with methylene chloride dried (MgSO4) the solvent was evaporated in vacuo to an oil residue which triturated with 1-chlorobutane