반응 #466882

반응 방정식

N,N-diethyl-2-(4-aminophenoxy)ethylamine

2,6-dimethoxybenzoic acid chloride

→

4′-[2-(diethylamino)ethoxy]-2,6-dimethoxybenzanilide

수율 70.0%

용매

pyridine

반응 조건

후처리

1. 1
   농축the reaction mixture was concentrated under vacuum and residue
2. 2
   workup.DISSOLUTIONwas dissolved into chloroform (50 ml)
3. 3
   세척The solution was washed with 1N sodium hydroxide aqueous solution
4. 4
   workup.DISTILLATIONSolvent was distilled out
5. 5
   기타residue was purified by silica-gel column chromatography (chloroform:methanol=25:1)

실험 절차

N,N-diethyl-2-(4-aminophenoxy)ethylamine (4.00 g) was added into 2,6-dimethoxybenzoic acid chloride (4.20 g) in pyridine (40 ml) in an ice bath. After stirred for one hour at room temperature, the reaction mixture was concentrated under vacuum and residue was dissolved into chloroform (50 ml). The solution was washed with 1N sodium hydroxide aqueous solution followed by water and then saturated sodium chloride (50 ml, each). Solvent was distilled out and residue was purified by silica-gel column chromatography (chloroform:methanol=25:1) to obtain 4′-[2-(diethylamino)ethoxy]-2,6-dimethoxybenzanilide (5.01 g) as color-less crystal.

출처