반응 #49167

반응 방정식

ethyl acrylate

ethyl glycinate hydrochloride

sodium hydroxide

→

Diethyl2-azabutane-1,4-dicarboxylate

용매

water

반응 조건

후처리

1. 1
   기타was ascertained by TLC (19 h)
2. 2
   기타After 19 h which it was partitioned with dichloromethane (3×100 mL)
3. 3
   건조The organic layer was dried with anhydrous sodium sulfate
4. 4
   여과filtered
5. 5
   기타evaporated
6. 6
   workup.DISTILLATIONThe residue was distilled
7. 7
   기타to afford AA (28.8 g, 61%)

실험 절차

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%).

출처