반응 #2352

반응 방정식

m-phenylenediamine

citraconic anhydride

→

N,N'-(m-phenylene)bis citraconamic acid

수율 99.9%

용매

acetone

—

reagent

acetone

acetone

반응 조건

후처리

1. 1
   기타flushed with nitrogen
2. 2
   기타The flask was fitted with a reflux condenser, mechanical stirrer
3. 3
   workup.ADDITIONthe solution added dropwise over about 1 1/2 hours
4. 4
   온도The reaction mixture was refluxed for an additional hour
5. 5
   여과suction filtered

실험 절차

A 3-liter, 3-neck round bottom flask was charged with 54 g (0.5 mole) of m-phenylenediamine and 500 ml of reagent acetone and flushed with nitrogen. The flask was fitted with a reflux condenser, mechanical stirrer and thermocouple. A dropping funnel containing 112 g (1.0 mole) of citraconic anhydride in 500 ml of reagent acetone was attached and the solution added dropwise over about 1 1/2 hours with stirring as the temperature was allowed to rise to reflux the acetone. The reaction mixture was refluxed for an additional hour, cooled to room temperature and suction filtered to give 166 g of N,N'-(m-phenylene)bis citraconamic acid as shown by NMR analysis, as a tan mustard-colored solid melting at 152°-156° C.

출처