반응 #1812

반응 방정식

sarcosine benzyl ester

succinic anhydride

→

title compound

수율 86.3%

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

수율 86.3%

용매

toluene

반응 조건

후처리

1. 1
   온도was heated
2. 2
   온도to reflux for 3 h
3. 3
   온도cooled
4. 4
   여과filtered
5. 5
   농축the filtrate was concentrated
6. 6
   추출extracted with ethyl acetate
7. 7
   농축with concentrated hydrochloric
8. 8
   추출extracted with ethyl acetate
9. 9
   세척The organic phase was washed with water
10. 10
    건조dried (magnesium sulfate)
11. 11
    농축concentrated

실험 절차

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).

출처