反応 #2352

反応方程式

m-phenylenediamine

citraconic anhydride

→

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

収率 99.9%

溶媒

acetone

—

reagent

acetone

acetone

反応条件

後処理

1. 1
   その他flushed with nitrogen
2. 2
   その他The flask was fitted with a reflux condenser, mechanical stirrer
3. 3
   workup.ADDITIONthe solution added dropwise over about 1 1/2 hours
4. 4
   温度The reaction mixture was refluxed for an additional hour
5. 5
   ろ過suction filtered

実験手順

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.

出典