9-Benzyl-1-oxa-4,9-diazaspiro[5.5]undecan-3-one → 9-Benzyl-1-oxa-4,9-diazaspiro[5.5]undecane

HRID 876054

반응식

HRID 876054 반응식
[H-].[Al+3].[Li+].[H-].[H-].[H-].[CH2:7]([N:14]1[CH2:25][CH2:24][C:17]2([O:22][CH2:21][C:20](=O)[NH:19][CH2:18]2)[CH2:16][CH2:15]1)[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1>O1CCCC1>[CH2:7]([N:14]1[CH2:15][CH2:16][C:17]2([O:22][CH2:21][CH2:20][NH:19][CH2:18]2)[CH2:24][CH2:25]1)[C:8]1[CH:9]=[CH:10][CH:11]=[CH:12][CH:13]=1

참가 물질

4

반응물 2

HCID 205220419-Benzyl-1-oxa-4,9-diazaspiro[5.5]undecan-3-oneHCID 21226445Aluminium lithium hydride

생성물 1

HCID 357537449-Benzyl-1-oxa-4,9-diazaspiro[5.5]undecane수율 82.7%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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.

후처리

  1. temperatureAfter 1.25 hours of reflux the reaction
  2. customquenched with water (2.22 mL)
  3. filtrationThe remaining solids were filtered off
  4. concentrationthe filtrate was concentrated

출처 및 근거

ORD 기록
ord-2dcc43ea69014a0ebf47a4682f6e2514
출처 데이터셋
uspto-grants-2015_03
특허 번호
US08980903B2

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