Aluminium lithium hydride → HCID 21941442, compound
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]=1Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
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
- additionwas added slowly at 0° C
- additionAfter addition reaction mixture
- stirringwas stirred for 30 minutes
- customquenched with saturated NH4Cl
- additionIt was diluted with CHCl3
- filtrationfiltered
- washThe fitrate was washed with saturated brine solution
- dry with materialdried over anhydrous MgSO4
- filtrationIt was filtered
Sources & evidence
- ORD record
- ord-e59ef9eaaa344cf1849474682d5f3539
- Source dataset
- uspto-grants-2006_09
- Patent number
- US07112582B2
Reaction notes
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