Reaktion #166413

Reaktionsgleichung

lithium aluminum hydride

compound 399

9-benzyl-1-oxa-4,9-diazaspiro[5.5]undecan-3-one

→

compound 402

Ausbeute 82.7%

9-benzyl-1-oxa-4,9-diazaspiro[5.5]undecane

Ausbeute 82.7%

Lösungsmittel

tetrahydrofuran

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturAfter 1.25 hours of reflux the reaction
2. 2
   Sonstigequenched with water (2.22 mL)
3. 3
   FiltrationThe remaining solids were filtered off
4. 4
   Einengenthe filtrate was concentrated

Vorschrift

To a stirring mixture of lithium aluminum hydride (2.22 g, 58.5 mmol) in tetrahydrofuran (70 mL) was added compound 399 (3.60 g, 13.8 mmol), portionwise over three minutes. After 1.25 hours of reflux the reaction was cooled to room temperature and quenched with water (2.22 mL), then 1N NaOH (2.22 mL), then water (2×2.22 mL). The remaining solids were filtered off, and the filtrate was concentrated to give compound 402 (2.81 g, 82%). LCMS-ESI (POS), M/Z, M+1: Found 247.1, Calculated 247.2.

Quelle