反应 #10949

反应方程式

Ethyl 3-amino-2-(2-methyl-[1,3]dioxolan-2-yl)propionate

4-nitrophthalic anhydride

→

desired product

收率 83.2%

Ethyl 3-(5-nitro-1,3-dioxo-1,3-dihydro-isoindol-2-yl)-2-(2-methyl-[1,3]dioxolan-2-yl)propionate

收率 83.2%

溶剂

chloroform

反应条件

后处理

1. 1
   其他the solvent was evaporated
2. 2
   workup.DISTILLATIONby distilling under a reduced pressure
3. 3
   其他The residue was purified

实验过程

Ethyl 3-amino-2-(2-methyl-[1,3]dioxolan-2-yl)propionate (800 mg, 3.94 mmol) was dissolved in 15 mL of chloroform, and 4-nitrophthalic anhydride (988 mg, 4.33 mmol) was added to the obtained solution. The resulting mixture was then refluxed at 80° C. for 5 days. After the reaction was completed, the solvent was evaporated by distilling under a reduced pressure. The residue was purified by performing column chromatography (eluent: n-hexane/ethyl acetate=1/1) to obtain the desired product as a yellow solid (1.24 g, 83%). Rf=0.32 (n-hexane/ethyl acetate=1/1)

来源