Reaktion #2165561

Reaktionsgleichung

sodium bis(2-methoxyethoxy)aluminum hydride

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

sodium hydroxide

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title product

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

Lösungsmittel

toluene

toluene

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturThe reaction mixture was cooled with ice
2. 2
   Extraktionthe aqueous layer was extracted with toluene
3. 3
   Sonstigethe solvent of the combined organic layer was evaporated under reduced pressure

Vorschrift

A solution (65% toluene solution) of sodium bis(2-methoxyethoxy)aluminum hydride (1.65 kg, 3.5 eq.) in toluene (870 mL) was added to a solution of 7-amino-5-benzyl-4-oxo-7-methyl-5-azaspiro[2.4]heptane (348 g, 1.51 mmol) in toluene (2.62 L), and the mixture was stirred at an internal temperature of 60° C. for 1 hour. The reaction mixture was cooled with ice. Aqueous sodium hydroxide solution (5N) was added to the cooled mixture, and the aqueous layer was extracted with toluene. The thus-obtained organic layers were combined, and the solvent of the combined organic layer was evaporated under reduced pressure, to thereby yield the title product as brown oil (343 g, purity: 81.3%, yield: 100%).

Quelle