반응 #60483

반응 방정식

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

trifluoroacetic acid

dichloromethane

sodium hydrogencarbonate

→

title compound

수율 51.4%

4-[3-Piperazin-1-yl-4-(3,3,5,5-tetramethylcyclohexyl)phenyl]morpholine

수율 51.4%

용매

ethyl acetate

Ethyl acetate

반응 조건

후처리

1. 1
   세척The separated organic layer was washed with water and brine in that order
2. 2
   건조dried over anhydrous sodium sulfate
3. 3
   여과The desiccant was filtered off
4. 4
   농축the filtrate was concentrated under reduced pressure
5. 5
   기타The resultant residue was purified by silica gel column chromatography (ethyl acetate/heptane)

실험 절차

A mixture of 4-[5-morpholin-4-yl-2-(3,3,5,5-tetramethylcyclohexyl)phenyl]piperazine-1-carboxylic acid t-butyl ester (103 mg, 0.212 mmol) produced in Example (81d), trifluoroacetic acid (1 mL, 13.0 mmol) and dichloromethane (2 mL) was stirred for 1 hour at room temperature. Ethyl acetate and saturated aqueous solution of sodium hydrogencarbonate were 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 resultant residue was purified by silica gel column chromatography (ethyl acetate/heptane) to give 42 mg of the title compound as a colorless oil.

출처