反応 #60453

反応方程式

sodium carbonate

4-[4-bromo-2-(4,4-dimethylcyclohexyl)phenyl]piperazine-1-carboxylic acid t-butyl ester

trifluoroacetic acid

dichloromethane

→

crude product

収率 103.7%

1-[4-Bromo-2-(4,4-dimethylcyclohexyl)phenyl]piperazine

収率 103.7%

溶媒

ethyl acetate

反応条件

後処理

1. 1
   洗浄The separated organic layer was washed with water and brine in that order
2. 2
   乾燥dried over anhydrous sodium sulfate
3. 3
   ろ過The desiccant was filtered off
4. 4
   濃縮the filtrate was concentrated under reduced pressure
5. 5
   その他The residue was dried under reduced pressure

実験手順

A mixture of 4-[4-bromo-2-(4,4-dimethylcyclohexyl)phenyl]piperazine-1-carboxylic acid t-butyl ester (1.5 g, 3.32 mmol) produced in Example (3e), trifluoroacetic acid (3 mL, 38.7 mmol) and dichloromethane (6 mL) was stirred for 2 hours and 30 minutes at room temperature. Saturated aqueous solution of sodium carbonate was added to the reaction mixture and extraction was performed with ethyl acetate. The separated organic layer was washed with water and brine in that order and then dried over anhydrous sodium sulfate. The desiccant was filtered off and the filtrate was concentrated under reduced pressure. The residue was dried under reduced pressure to give 1.21 g of a crude product of the title compound as a brown oil.

出典