Sodium sulfate decahydrate → HCID 2759476, compound

HRID 384129Notes

Reaction equation

HRID 384129 reaction equation
C[O:2][C:3](=O)[CH2:4][C:5]1[CH:10]=[CH:9][CH:8]=[C:7]([O:11][CH:12]([CH3:14])[CH3:13])[CH:6]=1.[H-].[Al+3].[Li+].[H-].[H-].[H-].O.O.O.O.O.O.O.O.O.O.S([O-])([O-])(=O)=O.[Na+].[Na+]>>[CH:12]([O:11][C:7]1[CH:6]=[C:5]([CH2:4][CH2:3][OH:2])[CH:10]=[CH:9][CH:8]=1)([CH3:14])[CH3:13]

Participants

4

Reactant 3

HCID 62649Sodium sulfate decahydrateHCID 15506060HCID 15506060, compoundHCID 21226445Aluminium lithium hydride

Product 1

HCID 2759476HCID 2759476, compound

Procedure

To a solution of methyl(3-isopropoxyphenyl)acetate (280 mg) in tetrahedron (5 ml), 52 mg of lithium aluminum hydride was added under ice-cooling, and the reaction solution was stirred at the same temperature for 25 minutes. To the reaction solution was added sodium sulfate decahydrate, and the mixture was stirred at room temperature for 2 hours. The reaction solution was filtered, and then the filtrate was distilled off under reduced pressure. The residue obtained was purified by silica gel column chromatography (eluent: ethyl acetate/hexane (0:100-50:50) to afford the title compound as a colorless oil.

Workup

  1. temperaturecooling
  2. stirringthe mixture was stirred at room temperature for 2 hours
  3. filtrationThe reaction solution was filtered
  4. distillationthe filtrate was distilled off under reduced pressure
  5. customThe residue obtained
  6. customwas purified by silica gel column chromatography (eluent

Sources & evidence

ORD record
ord-5a486fbbb81e4a119b57f95fd2021531
Source dataset
uspto-grants-2013_02
Patent number
US08367708B2

Reaction notes

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