Aluminium lithium hydride → HCID 21941442, compound

HRID 2216549Notes

Reaction equation

HRID 2216549 reaction equation
[H-].[H-].[H-].[H-].[Li+].[Al+3].[C:7]([N:15]1[CH2:20][CH2:19][C:18]2[S:21][C:22]([C:24](OCC)=[O:25])=[CH:23][C:17]=2[CH2:16]1)(=O)[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1>C1COCC1>[CH2:7]([N:15]1[CH2:20][CH2:19][C:18]2[S:21][C:22]([CH2:24][OH:25])=[CH:23][C:17]=2[CH2:16]1)[C:8]1[CH:9]=[CH:10][CH:11]=[CH:12][CH:13]=1

Participants

4

Procedure

To stirred suspension of LAH (2.0 gms) a solution of ethyl 5-benzoyl-4,5,6,7-tetrahydrothieno[3,2-c]pyridine-2-carboxylate (6.0 g, 19 mmol) in THF was added slowly at 0° C. After addition reaction mixture was stirred for 30 minutes and quenched with saturated NH4Cl. It was diluted with CHCl3 and filtered. The fitrate was washed with saturated brine solution and dried over anhydrous MgSO4. It was filtered and taken to next step with out purifications. Yield: 4.5 g 91%. Yellow liquid.

Workup

  1. additionwas added slowly at 0° C
  2. additionAfter addition reaction mixture
  3. stirringwas stirred for 30 minutes
  4. customquenched with saturated NH4Cl
  5. additionIt was diluted with CHCl3
  6. filtrationfiltered
  7. washThe fitrate was washed with saturated brine solution
  8. dry with materialdried over anhydrous MgSO4
  9. filtrationIt was filtered

Sources & evidence

ORD record
ord-e59ef9eaaa344cf1849474682d5f3539
Source dataset
uspto-grants-2006_09
Patent number
US07112582B2

Reaction notes

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