반응 #1789680

반응 방정식

CO2

hydrogen chloride

m-chloroaniline

2-oxazolidinone

m-chloroaniline hydrochloride

→

N-(3-chlorophenyl)-1,2-ethanediamine

수율 80.0%

용매

water

ether

반응 조건

후처리

1. 1
   기타by grinding with a mortar and pestle
2. 2
   workup.ADDITIONThe ground mixture was then added to a 250 ml flask
3. 3
   기타equipped with a mechanical stirrer
4. 4
   온도Heating
5. 5
   온도was cooled
6. 6
   여과filtered
7. 7
   기타to separate
8. 8
   추출Extraction with methylene chloride
9. 9
   기타drying
10. 10
    workup.DISTILLATIONdistillation under vacuum

실험 절차

Gaseous hydrogen chloride was reacted with m-chloroaniline in ether at 0° C. to prepare the m-chloroaniline hydrochloride. This reactant (65.6 g, 0.4 mole) was then intimately mixed with 2-oxazolidinone by grinding with a mortar and pestle. The ground mixture was then added to a 250 ml flask equipped with a mechanical stirrer and gas vent. The flask was heated in an oil bath to 160° C. with stirring. The solid mixture melted and CO2 evolution commenced in about 15 minutes. Heating was continued for about six hours whereupon the flask was cooled and the contents dissolved in water and filtered. The filtrate was then basified with aqueous caustic causing a yellow oil to separate. Extraction with methylene chloride, drying and distillation under vacuum gave 55 g (80 percent yield) of N-(3-chlorophenyl)-1,2-ethanediamine.

출처