反应 #1812

反应方程式

sarcosine benzyl ester

succinic anhydride

→

title compound

收率 86.3%

N-(3-Carboxypropanoyl)-N-methyl-glycine Benzyl Ester

收率 86.3%

溶剂

toluene

反应条件

后处理

1. 1
   温度was heated
2. 2
   温度to reflux for 3 h
3. 3
   温度cooled
4. 4
   过滤filtered
5. 5
   浓缩the filtrate was concentrated
6. 6
   萃取extracted with ethyl acetate
7. 7
   浓缩with concentrated hydrochloric
8. 8
   萃取extracted with ethyl acetate
9. 9
   洗涤The organic phase was washed with water
10. 10
    干燥dried (magnesium sulfate)
11. 11
    浓缩concentrated

实验过程

A mixture of sarcosine benzyl ester (3.0 g, 30.7 mmol) and succinic anhydride (5.5 g, 30.7 mmol) in toluene (75 mL) was heated to reflux for 3 h, cooled, filtered, and the filtrate was concentrated. The residue was taken up in 5% aqueous sodium carbonate and extracted with ethyl acetate. The aqueous phase was adjusted to pH 3 with concentrated hydrochloric using Congo Red paper and extracted with ethyl acetate. The organic phase was washed with water, dried (magnesium sulfate) and concentrated to yield the title compound (7.4 g, 67.5%): TLC Rf 0.48 (silica, 9:1:1 dichloromethane:methanol:formic acid).

来源