反应详情

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).

1. temperaturewas heated
2. temperatureto reflux for 3 h
3. temperaturecooled
4. filtrationfiltered
5. concentrationthe filtrate was concentrated
6. extractionextracted with ethyl acetate
7. concentrationwith concentrated hydrochloric
8. extractionextracted with ethyl acetate
9. washThe organic phase was washed with water
10. dry with materialdried (magnesium sulfate)
11. concentrationconcentrated