Sodium sulfate decahydrate → 2-(4-Benzylpiperazin-1-yl)ethan-1-amine

HRID 1162342Notes

Reaction equation

HRID 1162342 reaction equation
[H-].[Al+3].[Li+].[H-].[H-].[H-].[CH2:7]([N:14]1[CH2:19][CH2:18][N:17]([CH2:20][C:21]#[N:22])[CH2:16][CH2:15]1)[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1.O.O.O.O.O.O.O.O.O.O.S([O-])([O-])(=O)=O.[Na+].[Na+]>C1COCC1>[CH2:7]([N:14]1[CH2:15][CH2:16][N:17]([CH2:20][CH2:21][NH2:22])[CH2:18][CH2:19]1)[C:8]1[CH:9]=[CH:10][CH:11]=[CH:12][CH:13]=1

Participants

5

Reactant 3

HCID 62649Sodium sulfate decahydrateHCID 38557212-(4-Benzylpiperazin-1-yl)acetonitrileHCID 21226445Aluminium lithium hydride

Product 1

HCID 27353312-(4-Benzylpiperazin-1-yl)ethan-1-amineYield 95%

Reagents, catalysts & solvents 1

HCID 8028TetrahydrofuranSolvent3×

Procedure

To a suspension of lithium aluminum hydride (5.0 g) in anhydrous THF (150 ml) was added a solution of (4-benzyl-1-piperazinyl)acetonitrile (11 g) obtained in Example 95a) in anhydrous THF (50 ml) under ice-cooling. The reaction solution was refluxed for 3 hours, to the reaction solution was then added sodium sulfate decahydrate (420 g) under ice-cooling, and mixed for 15 hours. The reaction solution was diluted with THF, the precipitate obtained by decantation was filtered off, and the solvent was distilled off under reduced pressure to obtain the title compound as pale yellow liquid (10 g, 95%).

Workup

  1. temperaturecooling
  2. temperatureThe reaction solution was refluxed for 3 hours, to the reaction solution
  3. additionmixed for 15 hours
  4. customthe precipitate obtained by decantation
  5. filtrationwas filtered off
  6. distillationthe solvent was distilled off under reduced pressure

Sources & evidence

ORD record
ord-b8dd6ce48ac149cba9524242005e5ca5
Source dataset
uspto-grants-2010_10
Patent number
US07820673B2

Reaction notes

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