反応 #1269838

反応方程式

ethyl acrylate

ethyl glycinate hydrochloride

sodium hydroxide

→

Diethyl-2-azabutane-1,4-dicarboxylate

溶媒

water

反応条件

後処理

1. 1
   その他After 19 h the solution is partitioned with dichloromethane (3×100 mL)
2. 2
   乾燥The organic layer is dried with anhydrous sodium sulfate
3. 3
   ろ過filtered
4. 4
   その他evaporated
5. 5
   workup.DISTILLATIONThe residue is distilled
6. 6
   その他to afford AA (28.8 g, 61%)

実験手順

A 4.7 M aqueous solution of sodium hydroxide (50 mL) is added into a stirred, ice-cooled solution of ethyl glycinate hydrochloride (32.19 g, 0.23 mole) in water (50 mL). Then, ethyl acrylate (23.1 g, 0.23 mole) is added and the mixture is stirred at room temperature until completion of the reaction is ascertained by TLC. After 19 h the solution is partitioned with dichloromethane (3×100 mL). The organic layer is dried with anhydrous sodium sulfate, filtered and evaporated. The residue is distilled to afford AA (28.8 g, 61%).

出典