反応 #49167

反応方程式

ethyl acrylate

ethyl glycinate hydrochloride

sodium hydroxide

→

Diethyl2-azabutane-1,4-dicarboxylate

溶媒

water

反応条件

後処理

1. 1
   その他was ascertained by TLC (19 h)
2. 2
   その他After 19 h which it was partitioned with dichloromethane (3×100 mL)
3. 3
   乾燥The organic layer was dried with anhydrous sodium sulfate
4. 4
   ろ過filtered
5. 5
   その他evaporated
6. 6
   workup.DISTILLATIONThe residue was distilled
7. 7
   その他to afford AA (28.8 g, 61%)

実験手順

A 4.7M aqueous solution of sodium hydroxide (50 mL) was 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) was added and the mixture was stirred at room temperature until the completion of reaction was ascertained by TLC (19 h). After 19 h which it was partitioned with dichloromethane (3×100 mL). The organic layer was dried with anhydrous sodium sulfate, filtered and evaporated. The residue was distilled to afford AA (28.8 g, 61%).

出典