反応 #170684

反応方程式

itaconic acid

2,4-dimethoxybenzylamine

→

titled compound

収率 90.6%

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

収率 90.6%

溶媒

toluene

toluene

反応条件

後処理

1. 1
   温度at reflux
2. 2
   濃縮concentrated under reduced pressure
3. 3
   workup.ADDITIONTo the resulting residue was added diethyl ether (600 ml)
4. 4
   workup.STIRRINGthe mixture was stirred
5. 5
   ろ過The precipitated solid was collected by filtration
6. 6
   洗浄washed with diethyl ether
7. 7
   乾燥a small amount of ethyl acetate, and then dried under reduced pressure

実験手順

To a solution of itaconic acid (65.3 g) in toluene (400 ml) was added a solution of 2,4-dimethoxybenzylamine (84.0 g) in toluene (100 ml), and the mixture was stirred for 15 hours at reflux. This reaction solution was cooled to room temperature, and concentrated under reduced pressure. To the resulting residue was added diethyl ether (600 ml), and the mixture was stirred. The precipitated solid was collected by filtration, washed with diethyl ether and a small amount of ethyl acetate, and then dried under reduced pressure to give the titled compound (127 g).

出典