反应详情

Icosanedioic acid tert-butyl ester 2,5-dioxo-pyrrolidin-1-yl ester (6.01 g, 12.124 mmol) was dissolved in THF (150 mL) and mixed with a slurry of H-Glu-OtBu (2.71 g, 13.33 mmol) in DMF/water (1/1, 40 mL). This resulted in a gel-like solution which was heated to give a clear solution that was stirred at RT for 3 h. Then the solution was evaporated, 100 mL of water was added and the mixture was heated to 60° C. which resulted in a solution which crystallised on cooling. The precipitate was recrystallised from acetonitrile and the crystals were dried in vacuum. Yield 6.82 g (96%).

1. customThis resulted in a gel-like solution which
2. temperaturewas heated
3. customto give a clear solution that
4. customThen the solution was evaporated
5. addition100 mL of water was added
6. temperaturethe mixture was heated to 60° C. which
7. customresulted in a solution which
8. customcrystallised
9. temperatureon cooling
10. customThe precipitate was recrystallised from acetonitrile
11. customthe crystals were dried in vacuum