반응 #1211

반응 방정식

KOH

N2

N,N-bis(2-hydroxyethyl)-16-hydroxyhexadecanamide

LiAlH4

→

title compound

수율 62.0%

16-[N,N-bis(2-hydroxyethyl)amino]-1-hexadecanol

수율 62.0%

용매

tetrahydrofuran

반응 조건

후처리

1. 1
   기타A 500-ml flask equipped with a stirrer
2. 2
   온도reflux condenser
3. 3
   workup.ADDITIONwere added
4. 4
   온도After cooling the reaction mixture to room temperature
5. 5
   기타a salt deposited was separated by filtration
6. 6
   workup.DISTILLATIONThe solvent was then distilled off under reduced pressure
7. 7
   기타the resultant residue was purified by column chromatography on silica gel

실험 절차

A 500-ml flask equipped with a stirrer and reflux condenser was charged with 3.01 g (79.3 mmol) of LiAlH4 and 200 ml of tetrahydrofuran. While stirring the mixture at room temperature in an N2 atmosphere, 5.00 g (13.9 mmol) of N,N-bis(2-hydroxyethyl)-16-hydroxyhexadecanamide were added, followed by stirring at 65° C. for 18 hours. After cooling the reaction mixture to room temperature, 15 g of 3% aqueous KOH were added, and a salt deposited was separated by filtration. The solvent was then distilled off under reduced pressure, and the resultant residue was purified by column chromatography on silica gel, thereby obtaining 2.98 g (yield: 62%) of the title compound (IId-3).

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