تفاعل #60465

معادلة التفاعل

sodium hydrogencarbonate

4-[4-methyl-2-(3,3,5,5-tetramethylcyclohexyl)phenyl]piperazine-1-carboxylic acid t-butyl ester

trifluoroacetic acid

dichloromethane

→

title compound

المردود 90.4%

1-[4-Methyl-2-(3,3,5,5-tetramethylcyclohexyl)phenyl]piperazine

المردود 90.4%

المذيبات

ethyl acetate

ظروف التفاعل

المعالجة

1. 1
   تركيزThe separated organic layer was concentrated under reduced pressure
2. 2
   أخرىThe resultant residue was purified by NH silica gel column chromatography (ethyl acetate/hexane)

الإجراء التجريبي

A mixture of 4-[4-methyl-2-(3,3,5,5-tetramethylcyclohexyl)phenyl]piperazine-1-carboxylic acid t-butyl ester (124 mg, 0.299 mmol) produced in Example (70a), trifluoroacetic acid (1 mL, 12.9 mmol) and dichloromethane (2 mL) was stirred for 2 hours and 30 minutes at room temperature. Saturated aqueous solution of sodium hydrogencarbonate was added to the reaction mixture and extraction was performed with ethyl acetate. The separated organic layer was concentrated under reduced pressure. The resultant residue was purified by NH silica gel column chromatography (ethyl acetate/hexane) to give 85 mg of the title compound as yellow crystals.

المصدر