S-乙酰硫基乙酸

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

实验步骤: S-Acetyl-2-mercaptoacetic acid (75 mmoles) and N-hydroxysuccinimide (75 mmoles), were dissolved in 150 ml dioxane and reacted with cooling in ice with N,N'-dicyclohexylcarbodiimide (75 mmoles) and the mixture was kept at 4° C. for 16 h. The N,N'-dicyclohexylurea formed was removed by filtration and the solvent evaporated in vacuo. The residue was twice recrystallized from 2-propanol. reacted

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

实验步骤: S-Acetyl-2-mercaptoacetic acid (75 mmoles) and N-hydroxysuccinimide (75 mmoles), were dissolved in 150 ml dioxane and reacted with cooling in ice with N,N'-dicyclohexylcarbodiimide (75 mmoles) and the mixture was kept at 4° C. for 16 h. The N,N'-dicyclohexylurea formed was removed by filtration and the solvent evaporated in vacuo. The residue was twice recrystallized from 2-propanol. reacted

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

实验步骤: 2.94 g of 3-{3-(piperidinomethyl)phenoxy}propylamine was dissolved in 80 ml of dichloromethane, and stirred under cooling in an ice bath. 1.60 g of 2-(acetylthio)acetic acid and 2.26 g of EDC were added to this solution, and stirred at 0° C. for 30 minutes then at room temperature overnight. 100 ml of water and 50 ml of dichloromethane were added to the reaction solution, and extraction was carried out. The dichloromethane layer was washed twice with water, and dried over anhydrous magnesium sulfate. The solvent was evaporated in vacuo, and the residue was purified by silica gel column chromatography using methanol:dichloromethane=1:15 as developing solvent to obtain the colorless oily N-[3-{3-(piperidinomethyl)phenoxy}propyl]-2-(acetylthio)acetamide. Yield: 2.23 g. under cooling in an ice bath stirred at 0° C. for 30 minutes at room temperature overnight The dichloromethane layer was washed twice with water dried over anhydrous magnesium sulfate The solvent was evaporated in vacuo the residue was purified by silica gel column chromatography

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

实验步骤: S-Acetyl-2-mercaptoacetic acid (75 mmoles) and N-hydroxysuccinimide (75 mmoles), were dissolved in 150 ml dioxane and reacted with cooling in ice with N,N'-dicyclohexylcarbodiimide (75 mmoles) and the mixture was kept at 4° C. for 16 h. The N,N'-dicyclohexylurea formed was removed by filtration and the solvent evaporated in vacuo. The residue was twice recrystallized from 2-propanol. reacted