반응 #488173

반응 방정식

N-Boc-Asp(O-t-Bu)OH

Boc2O

ammonium bicarbonate

dimethylformamide

→

title compound

tert-butyl (3S)-4-amino-3-[(tert-butoxycarbonyl)amino]-4-oxobutanoate

용매

pyridine

toluene

water

반응 조건

후처리

1. 1
   workup.ADDITIONwas added dropwise
2. 2
   workup.ADDITIONwere added to the reaction solution
3. 3
   workup.STIRRINGstirred for 30 minutes
4. 4
   기타to separate the layers
5. 5
   기타The organic layer thus obtained
6. 6
   workup.DISTILLATIONwas distilled under reduced pressure
7. 7
   기타to remove t-butanol and toluene

실험 절차

360.0 g of the starting material, N-Boc-Asp(O-t-Bu)OH, together with Boc2O (353.0 g) and ammonium bicarbonate (NH4HCO3, 123.9 g) was added to dimethylformamide (1174.6 g), and pyridine (61.0 g) was added dropwise thereto at room temperature, and the reaction mixture was then stirred for about 3 hours. Upon completion of the reaction, water (1440 ml) and toluene (1800 ml) were added to the reaction solution and stirred for 30 minutes to separate the layers. The organic layer thus obtained was distilled under reduced pressure to remove t-butanol and toluene to obtain the title compound, which was directly used in the next reaction.

출처