Aluminium lithium hydride → HCID 21050991, compound

HRID 914976Notes

Reaction equation

HRID 914976 reaction equation
[NH2:1][C:2]([CH3:16])([CH3:15])[C:3]([N:5]1[CH2:14][CH2:13][C:12]2[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=2)[CH2:6]1)=O.[H-].[H-].[H-].[H-].[Li+].[Al+3]>C1COCC1>[CH2:6]1[C:7]2[C:12](=[CH:11][CH:10]=[CH:9][CH:8]=2)[CH2:13][CH2:14][N:5]1[CH2:3][C:2]([NH2:1])([CH3:15])[CH3:16]

Participants

4

Reactant 2

HCID 21226445Aluminium lithium hydrideHCID 28263565HCID 28263565, compound

Product 1

HCID 21050991HCID 21050991, compoundYield 79%

Reagents, catalysts & solvents 1

HCID 8028TetrahydrofuranSolvent

Procedure

To a solution of 42 (0.20 g, 0.91 mmol) in anhydrous THF (4 mL) at 0° C. was added LiAlH4 (1.0 M in THF, 3.0 mL, 3.0 mmol). The resulting mixture was heated under reflux overnight before it was allowed to cool to room temperature. Excess LiAlH4 was destroyed with slow addition of Na2SO4.10H2O at 0° C. until gas evolution ceased. The solids were filtered off and the filtrate was concentrated to give 43 (0.14 g, 79%).

Workup

  1. temperatureThe resulting mixture was heated
  2. temperatureunder reflux overnight before it
  3. customExcess LiAlH4 was destroyed with slow addition of Na2SO4.10H2O at 0° C. until gas evolution
  4. filtrationThe solids were filtered off
  5. concentrationthe filtrate was concentrated

Sources & evidence

ORD record
ord-e650b9c75bb447ba8e6c959660e471ba
Source dataset
uspto-grants-2007_09
Patent number
US07265122B2

Reaction notes

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