Aluminium lithium hydride → HCID 22998673, compound

HRID 854027Notes

Reaction equation

HRID 854027 reaction equation
[H-].[Al+3].[Li+].[H-].[H-].[H-].[C:7]1([C:30]2[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=2)[CH:12]=[CH:11][C:10]([CH2:13][O:14][C:15]2[CH:16]=[C:17]3[C:22](=[CH:23][CH:24]=2)[CH2:21][CH:20]([CH2:25][C:26](OC)=[O:27])[CH2:19][CH2:18]3)=[CH:9][CH:8]=1>C1COCC1.[C@H](O)(C([O-])=O)[C@@H](O)C([O-])=O.[Na+].[K+]>[C:7]1([C:30]2[CH:31]=[CH:32][CH:33]=[CH:34][CH:35]=2)[CH:8]=[CH:9][C:10]([CH2:13][O:14][C:15]2[CH:16]=[C:17]3[C:22](=[CH:23][CH:24]=2)[CH2:21][CH:20]([CH2:25][CH2:26][OH:27])[CH2:19][CH2:18]3)=[CH:11][CH:12]=1

Participants

5

Reactant 2

HCID 21226445Aluminium lithium hydrideHCID 54014545HCID 54014545, compound

Product 1

HCID 22998673HCID 22998673, compoundYield 99.3%

Reagents, catalysts & solvents 2

HCID 8028TetrahydrofuranSolvent2×HCID 9357Potassium Sodium TartrateSolvent

Procedure

To a suspension of lithium aluminum hydride (4.71 g) in THF (200 ml) was added a solution of methyl 6-(4-biphenylyl)methoxy-2-tetralinacetate (24.0 g) in THF (50 ml) under ice-cooling. The reaction mixture was stirred at room temperature for 2 hr and diluted with saturated aqueous Rochelle salt. The precipitate was filtered off and the filtrate was concentrated. The residue was recrystallized from ethyl acetate-hexane to obtain the titled compound (22.1 g).

Workup

  1. temperaturecooling
  2. filtrationThe precipitate was filtered off
  3. concentrationthe filtrate was concentrated
  4. customThe residue was recrystallized from ethyl acetate-hexane

Sources & evidence

ORD record
ord-cc98681659c84835aeaf5938ef74308d
Source dataset
uspto-grants-2007_08
Patent number
US07256204B2

Reaction notes

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