반응 #164610

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4-(2,6-difluoro-4-nitro-phenyl)-piperazine-1-carboxylic acid tert-butyl ester

Intermediate II

4-(2,6-difluoro-4-nitro-phenyl)-piperazine-1-carboxylic acid tert-butyl ester

→

title compound

수율 95.0%

4-(4-Amino-2,6-difluoro-phenyl)-piperazine-1-carboxylic acid tert-butyl ester

수율 95.0%

용매

methanol

반응 조건

후처리

1. 1
   기타Flask was evacuated
2. 2
   workup.ADDITIONhydrogen was introduced with the help of balloon
3. 3
   여과On completion, the reaction mixture was filtered through celite pad
4. 4
   기타The filterate was evaporated

실험 절차

To a solution of 4-(2,6-difluoro-4-nitro-phenyl)-piperazine-1-carboxylic acid tert-butyl ester (Intermediate II) (30 g, 0.09 mol), in methanol (500 mL) under argon atmosphere was added 10% Pd/C (4.5 g, 15 mol% by weight). Flask was evacuated and hydrogen was introduced with the help of balloon. The reaction mixture was stirred under hydrogen and progress of the reaction was monitored by TLC. On completion, the reaction mixture was filtered through celite pad using methanol as solvent. The filterate was evaporated to provide title compound (26 g, 95%) as pale yellow solid.

출처