反応 #87166

反応方程式

itaconic acid

2,4-dimethoxybenzylamine

→

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

収率 71.6%

溶媒

toluene

toluene

反応条件

後処理

1. 1
   温度under reflux
2. 2
   濃縮concentrated under reduced pressure
3. 3
   workup.ADDITIONThe residue was treated with diethyl ether (100 mL)
4. 4
   ろ過the resulting precipitate was collected by filtration
5. 5
   洗浄washed with diethyl ether and EtOAc
6. 6
   その他dried

実験手順

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.

出典