반응 #2550

반응 방정식

4-chloromethyl-N-(2-methoxyphenyl)benzamide

dimethylamine

→

title compound

수율 100.0%

N-(2-Methoxyphenyl)-4-dimethylaminomethylbenzamide

수율 100.0%

용매

dioxane

반응 조건

후처리

1. 1
   기타equipped with a cold finger
2. 2
   기타subsequent removal of dioxane
3. 3
   기타by evaporation
4. 4
   workup.ADDITIONthe resulting residue was diluted with ethyl acetate (30 ml)
5. 5
   건조The thus diluted solution was dried on anhydrous sodium carbonate
6. 6
   기타the resulting residue was purified

실험 절차

In an atmosphere of argon, 4-chloromethyl-N-(2-methoxyphenyl)benzamide (276 mg, 1.0 mmol) was put into a 25 ml capacity eggplant type flask equipped with a cold finger and dissolved in dioxane (3 ml), followed by the addition of 50% dimethylamine aqueous solution (3 ml) at room temperature. After 2.5 hours of stirring at 80° C. and subsequent removal of dioxane by evaporation, the resulting residue was diluted with ethyl acetate (30 ml). The thus diluted solution was dried on anhydrous sodium carbonate, and the resulting residue was purified by subjecting it to a silica gel column chromatography (ether-ethyl acetate-ethyl acetate:methanol=10:1) to obtain 284 mg (100%) of the title compound in the form of colorless oil.

출처