반응 #2355147

반응 방정식

sodium hydroxide

N-(2-methylindol-3-ylacetyl)-N′-[bis(4-fluorophenyl)methyl]piperazine

lithium aluminum hydride

water

→

N-(2-methylindol-3-ylethyl)-N′-[bis(4-fluorophenyl)methyl]piperazine

수율 52.4%

용매

tetrahydrofuran

tetrahydrofuran

반응 조건

후처리

1. 1
   workup.ADDITIONUpon completion of the addition the reaction mixture
2. 2
   온도was heated
3. 3
   온도to reflux
4. 4
   온도The solution was warmed to ambient temperature
5. 5
   추출extracted with ethyl acetate
6. 6
   건조The extract was dried with sodium sulfate
7. 7
   여과filtered
8. 8
   농축The filtrate was concentrated under reduced pressure

실험 절차

A solution of 1.5 grams (0.003 mole) of N-(2-methylindol-3-ylacetyl)-N′-[bis(4-fluorophenyl)methyl]piperazine in 10.0 mL of anhydrous tetrahydrofuran was added to a stirred mixture of 0.4 gram (0.010 mole) of lithium aluminum hydride in 5.0 mL of anhydrous tetrahydrofuran. Upon completion of the addition the reaction mixture was heated to reflux, where it stirred for 2.5 hours. The reaction mixture was cooled to 0° C., and water was added, followed by 50 mL of aqueous 10% sodium hydroxide. The solution was warmed to ambient temperature and then extracted with ethyl acetate. The extract was dried with sodium sulfate and filtered. The filtrate was concentrated under reduced pressure, yielding 0.7 gram of N-(2-methylindol-3-ylethyl)-N′-[bis(4-fluorophenyl)methyl]piperazine, mp 65-73° C. The NMR spectrum was consistent with the proposed structure.

출처