반응 #166413

반응 방정식

lithium aluminum hydride

compound 399

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

→

compound 402

수율 82.7%

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

수율 82.7%

용매

tetrahydrofuran

반응 조건

후처리

1. 1
   온도After 1.25 hours of reflux the reaction
2. 2
   기타quenched with water (2.22 mL)
3. 3
   여과The remaining solids were filtered off
4. 4
   농축the filtrate was concentrated

실험 절차

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.

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