تفاعل #1080222

معادلة التفاعل

water

n-butyl 4-[[2-oxo-4-(piperidin-4-yl)-piperazin-1-yl]acetyl]phenoxyacetate dihydrochloride

proton sponge

1-chloroethyl chloroformate

→

n-butyl 4-[[4-[1-(1-chloroethyl)oxycarbonylpiperidin-4-yl]-2-oxopiperazin-1-yl]acetyl]phenoxyacetate

المذيبات

methylene chloride

ظروف التفاعل

المعالجة

1. 1
   أخرىsynthesized
2. 2
   workup.STIRRINGthe mixture was stirred at room temperature for 18 hours
3. 3
   أخرىThe reaction mixture thus obtained
4. 4
   استخلاصextracted three times with 4 ml of ethyl acetate
5. 5
   أخرىThe organic layer collected
6. 6
   تجفيفwas dried over magnesium sulfate
7. 7
   أخرىthe solvent was removed by distillation

الإجراء التجريبي

To a suspension of 99.6 mg of n-butyl 4-[[2-oxo-4-(piperidin-4-yl)-piperazin-1-yl]acetyl]phenoxyacetate dihydrochloride synthesized according to the method described in WO962503 in 2 ml of methylene chloride were added 151 mg of proton sponge and 26 μl of 1-chloroethyl chloroformate with stirring at 0° C., and the mixture was stirred at room temperature for 18 hours. The reaction mixture thus obtained was poured into 2 ml of water, and extracted three times with 4 ml of ethyl acetate. The organic layer collected was dried over magnesium sulfate, and the solvent was removed by distillation to give 82.7 mg of n-butyl 4-[[4-[1-(1-chloroethyl)oxycarbonylpiperidin-4-yl]-2-oxopiperazin-1-yl]acetyl]phenoxyacetate as a crude crystalline product.

المصدر