反応 #164610

反応方程式

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

収率 95.0%

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

収率 95.0%

溶媒

methanol

反応条件

後処理

1. 1
   その他Flask was evacuated
2. 2
   workup.ADDITIONhydrogen was introduced with the help of balloon
3. 3
   ろ過On completion, the reaction mixture was filtered through celite pad
4. 4
   その他The filterate was evaporated

実験手順

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.

出典