تفاعل #80373

معادلة التفاعل

2-mercaptoethanol

potassium hydroxide

N-[3-(4-piperidinomethyl-2-pyridyloxy)propyl]-2-chloroacetamide

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title compound

المردود 77.0%

N-[3-(4-Piperidinomethyl-2-pyridyloxy)propyl]-2-(2-hydroxyethylthio)acetamide

المردود 77.0%

المذيبات

methanol

ظروف التفاعل

المعالجة

1. 1
   تركيزAt the end of this time, the reaction mixture was concentrated by evaporation under reduced pressure
2. 2
   workup.ADDITIONthe concentrate was mixed with water
3. 3
   استخلاصthe resulting aqueous mixture was extracted with chloroform
4. 4
   تركيزThe extract was concentrated by evaporation under reduced pressure
5. 5
   أخرىthe residue was purified by column chromatography through silica gel
6. 6
   workup.ADDITIONby volume mixture of ethanol and chloroform as the eluent

الإجراء التجريبي

0.12 ml of 2-mercaptoethanol was added to a solution of 0.13 g of 85% potassium hydroxide and 0.50 g of N-[3-(4-piperidinomethyl-2-pyridyloxy)propyl]-2-chloroacetamide [prepared as described in step (a) above] in 10 ml methanol, and the resulting mixture was stirred at room temperature for 1 hour. At the end of this time, the reaction mixture was concentrated by evaporation under reduced pressure, the concentrate was mixed with water, and the resulting aqueous mixture was extracted with chloroform. The extract was concentrated by evaporation under reduced pressure, and the residue was purified by column chromatography through silica gel, using a 1:9 by volume mixture of ethanol and chloroform as the eluent, to give 0.43 g (yield 77%) of the title compound as an oil.

المصدر