Reaktion #87166

Reaktionsgleichung

itaconic acid

2,4-dimethoxybenzylamine

→

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

Ausbeute 71.6%

Lösungsmittel

toluene

toluene

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturunder reflux
2. 2
   Einengenconcentrated under reduced pressure
3. 3
   workup.ADDITIONThe residue was treated with diethyl ether (100 mL)
4. 4
   Filtrationthe resulting precipitate was collected by filtration
5. 5
   Waschenwashed with diethyl ether and EtOAc
6. 6
   Sonstigedried

Vorschrift

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.

Quelle