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Water → 8-[(3,4-Dihydro-2-naphthalenyl)methyl]-1-phenyl-1,3,8-triazaspiro[4.5]decan-4-one

HRID 2072475
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HRID 2072475 반응식
[CH:1]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH2:4][CH2:3][C:2]=1[CH2:11][N:12]1[CH2:22][CH2:21][C:15]2([NH:19][CH:18]=[N:17][C:16]2=[O:20])[CH2:14][CH2:13]1.[H-].[Al+3].[Li+].[H-].[H-].[H-].O.[OH-].[Na+]>O1CCCC1>[CH:1]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH2:4][CH2:3][C:2]=1[CH2:11][N:12]1[CH2:22][CH2:21][C:15]2([N:19]([C:1]3[CH:10]=[CH:5][CH:4]=[CH:3][CH:2]=3)[CH2:18][NH:17][C:16]2=[O:20])[CH2:14][CH2:13]1
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참가 물질

6

반응물 4

HCID 962Water2회HCID 14798Sodium HydroxideHCID 21226445Aluminium lithium hydrideHCID 178517902HCID 178517902, 화합물

생성물 1

HCID 214082128-[(3,4-Dihydro-2-naphthalenyl)methyl]-1-phenyl-1,3,8-triazaspiro[4.5]decan-4-one

시약·촉매·용매 1

HCID 8028
Tetrahydrofuran
용매
2회

실험 절차

A solution of 8-[(3,4-dihydro-2-naphthalenyl)methyl]-1,3,8-triazaspiro[4.5]dec-2-en-4-one (5.0 g) in dry tetrahydrofuran (30 ml) is added dropwise to a slurry of lithium aluminum hydride (0.5 g) in tetrahydrofuran (60 ml). The resulting mixture is refluxed under nitrogen for 16 hours. The reaction mixture is cooled and treated, in order, with water (0.6 ml), 15% sodium hydroxide solution (0.6 ml), and water (1.8 ml). The resulting mixture is stirred for 30 minutes. The mixture is filtered and the solids washed with chloroform. The filtrate is washed with brine, dried over sodium sulfate, and concentrated to give the title compound.

후처리

  1. temperatureThe resulting mixture is refluxed under nitrogen for 16 hours
  2. temperatureThe reaction mixture is cooled
  3. filtrationThe mixture is filtered
  4. washthe solids washed with chloroform
  5. washThe filtrate is washed with brine
  6. dry with materialdried over sodium sulfate
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-fac05a3abd8748a39bc815f8aa185f54
출처 데이터셋
uspto-grants-1977_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04051248

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