Reaktion #476430

Reaktionsgleichung

Lithium aluminum hydride

7-Amino-5-benzyl-4-oxo-7-methyl-5-azaspiro[2.4]heptane

Water

sodium hydroxide

→

title product

Ausbeute 98.6%

7-Amino-5-benzyl-7-methyl-5-azaspiro[2.4]heptane

Ausbeute 98.6%

Lösungsmittel

Toluene

tetrahydrofuran

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturthe solution was cooled with ice
2. 2
   Sonstigewas returned to room temperature
3. 3
   Temperaturthe reaction mixture was cooled with ice
4. 4
   Temperaturto cooled mixture
5. 5
   Sonstigeto separate the organic layer
6. 6
   Waschenthe organic layer was washed with saturated brine
7. 7
   Trocknenby drying with sodium sulfate
8. 8
   SonstigeThe desiccant was removed through filtration
9. 9
   Einengenthe filtrate was concentrated under reduced pressure

Vorschrift

7-Amino-5-benzyl-4-oxo-7-methyl-5-azaspiro[2.4]heptane (27 g) was dissolved in anhydrous tetrahydrofuran (265 mL) in an argon atmosphere, and the solution was cooled with ice. Lithium aluminum hydride (13.3 g) was added thereto, and the mixture was returned to room temperature. After disappearance of the starting materials had been confirmed, the reaction mixture was cooled with ice. Water (200 mL) and 28% aqueous sodium hydroxide solution (70 mL) were added to cooled mixture, followed by stirring. Toluene was added to the mixture for extraction to separate the organic layer, and the organic layer was washed with saturated brine, followed by drying with sodium sulfate. The desiccant was removed through filtration, and the filtrate was concentrated under reduced pressure, to thereby yield the title product (24.7 g, yield: 98.6%).

Quelle