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Water → 1-Benzyl-3-ethylpiperazine

HRID 420554
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HRID 420554 반응식
[H-].[Al+3].[Li+].[H-].[H-].[H-].[CH2:7]([N:14]1[CH2:19][C:18](=O)[NH:17][CH:16]([CH2:21][CH3:22])[C:15]1=O)[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1.O.[OH-].[Na+]>C1COCC1.[Cl-].[Na+].O.C(OCC)(=O)C>[CH2:7]([N:14]1[CH2:19][CH2:18][NH:17][CH:16]([CH2:21][CH3:22])[CH2:15]1)[C:8]1[CH:9]=[CH:10][CH:11]=[CH:12][CH:13]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 962WaterHCID 14798Sodium HydroxideHCID 21226445Aluminium lithium hydrideHCID 222733891-Benzyl-3-ethylpiperazine-2,5-dione

생성물 1

HCID 220365411-Benzyl-3-ethylpiperazine

시약·촉매·용매 3

HCID 8028Tetrahydrofuran용매3회
HCID 8857
Ethyl Acetate
용매
HCID 57417360Sodium chloride; water용매

실험 절차

To a suspension of lithium aluminium hydride (0.87 g; 22.9 mmol) in anhydrous THF (20 ml) was added dropwise a solution of 1-benzyl-3-ethylpiperazine-2,5-dion (1.50 g; 6.46 mmol) in anhydrous THF (10 ml) under ice-cooling. After stirring at room temperature for 18 hours, a mixture of water (0.25 ml) and THF (5 ml) and 2N-aqueous sodium hydroxide solution (0.5 ml) were added dropwise sequentially under ice-cooling. The mixture was stirred at room temperature for 1 hour. After filtration of aluminium hydroxide, the filtrate was condensed under reduced pressure. To the residue were added ethyl acetate and brine to separate. The organic layer was dried over anhydrous sodium sulphate. The solvent was evaporated under reduced pressure to give 1-benzyl-3-ethylpiperazine as pale yellow oil (1.29 g; 98%).

후처리

  1. temperaturecooling
  2. additionwere added dropwise sequentially under ice-
  3. temperaturecooling
  4. stirringThe mixture was stirred at room temperature for 1 hour
  5. filtrationAfter filtration of aluminium hydroxide
  6. customcondensed under reduced pressure
  7. customto separate
  8. dry with materialThe organic layer was dried over anhydrous sodium sulphate
  9. customThe solvent was evaporated under reduced pressure

출처 및 근거

ORD 기록
ord-cb951f7796534bfdae1d0583b1caa986
출처 데이터셋
uspto-grants-2012_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08097610B2

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