반응 #87166

반응 방정식

itaconic acid

2,4-dimethoxybenzylamine

→

1-(2,4-dimethoxybenzyl)-5-oxopyrrolidine-3-carboxylic acid

수율 71.6%

용매

toluene

toluene

반응 조건

후처리

1. 1
   온도under reflux
2. 2
   농축concentrated under reduced pressure
3. 3
   workup.ADDITIONThe residue was treated with diethyl ether (100 mL)
4. 4
   여과the resulting precipitate was collected by filtration
5. 5
   세척washed with diethyl ether and EtOAc
6. 6
   기타dried

실험 절차

To a solution of itaconic acid (13.0 g, 100 mmol) in toluene (50 ml) was added a solution of 2,4-dimethoxybenzylamine (17.54 g, 105.0 mmol) in toluene (50 mL) and the reaction mixture was stirred for 15 h under reflux. The mixture was cooled to ambient temperature and then concentrated under reduced pressure. The residue was treated with diethyl ether (100 mL) and the resulting precipitate was collected by filtration, washed with diethyl ether and EtOAc and dried to afford 1-(2,4-dimethoxybenzyl)-5-oxopyrrolidine-3-carboxylic acid (20.0 g, 71% yield) as a colorless solid.

출처