Réaction #72432

Équation de réaction

Z-Glu(Nle-OBzl)-OBzl

ethanol

hydrogen

→

γ-Glu-Nle

Rendement 7.1%

Solvants

water

Water

Conditions de réaction

Traitement

1. 1
   Autrereaction
2. 2
   Autre(14 hours)
3. 3
   AutreThe palladium/carbon was removed from the reaction system through filtration
4. 4
   Concentrationthe resulting filtrate was concentrated under reduced pressure
5. 5
   AutreThe residue was recrystallized from a small amount of water and ethanol to thus give γ-Glu-Nle (0.29 g) as hygroscopic crystals
6. 6
   workup.DISSOLUTIONFurthermore, the crystals were dissolved in water (30 mL)

Mode opératoire

Z-Glu(Nle-OBzl)-OBzl (4.05 g) and 5% palladium on carbon (5% palladium/carbon, 0.40 g) were added to a mixed solution of ethanol (50 mL) and water (10 mL), and a catalytic reducing reaction was carried out at 50° C. overnight (14 hours) in a hydrogen gas atmosphere. Water (10 mL) was added to the reaction system in small portions during the reaction. The palladium/carbon was removed from the reaction system through filtration and the resulting filtrate was concentrated under reduced pressure. The residue was recrystallized from a small amount of water and ethanol to thus give γ-Glu-Nle (0.29 g) as hygroscopic crystals. Furthermore, the crystals were dissolved in water (30 mL) followed by the lyophilization of the solution to give γ-Glu-Nle (0.13 g, 0.50 mM) as a white powder. The characteristic values thereof will be given below:

Source