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Water → 1-Benzyl-3-ethylpiperazine

HRID 420554
ノート
印刷プレビュー

反応式

HRID 420554 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

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

生成物 1

HCID 220365411-Benzyl-3-ethylpiperazine

試薬・触媒・溶媒 3

HCID 8028Tetrahydrofuran溶媒3 回
HCID 8857
Ethyl Acetate
溶媒
HCID 57417360Sodium chloride; water溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-cb951f7796534bfdae1d0583b1caa986
出典データセット
uspto-grants-2012_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08097610B2

反応ノート

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