Sodium Sulfate → HCID 54382887, compound

HRID 1388297Notes

Reaction equation

HRID 1388297 reaction equation
[C:1]([NH:4][CH:5]1[CH2:13][C:12]2[C:7](=[CH:8][CH:9]=[CH:10][C:11]=2[O:14][CH2:15][S:16][CH3:17])[C:6]1=[O:18])(=O)[CH3:2].[H-].[H-].[H-].[H-].[Li+].[Al+3].[O-]S([O-])(=O)=O.[Na+].[Na+]>C1COCC1>[CH2:1]([NH:4][C@@H:5]1[CH2:13][C:12]2[C:7](=[CH:8][CH:9]=[CH:10][C:11]=2[O:14][CH2:15][S:16][CH3:17])[C@H:6]1[OH:18])[CH3:2]

Participants

5

Reactant 3

HCID 24436Sodium SulfateHCID 20470805HCID 20470805, compoundHCID 21226445Aluminium lithium hydride

Product 1

HCID 54382887HCID 54382887, compound

Reagents, catalysts & solvents 1

HCID 8028TetrahydrofuranSolvent2×

Procedure

The residue from Step D is dissolved in 50 ml of THF and added to 3.8 g (0.1 m) of LiAlH4 in 50 ml of THF dropwise. The mixture is refluxed for one hour after completion of the addition. The mixture is cooled and sufficient saturated aqueous Na2SO4 solution is added to quench the excess LiAlH4. Methylene chloride and solid anhydrous Na2SO4 is added and the mixture is filtered. Concentration provides the crude product.

Workup

  1. temperatureThe mixture is refluxed for one hour
  2. additionafter completion of the addition
  3. temperatureThe mixture is cooled
  4. customto quench the excess LiAlH4
  5. additionMethylene chloride and solid anhydrous Na2SO4 is added
  6. filtrationthe mixture is filtered
  7. concentrationConcentration

Sources & evidence

ORD record
ord-b16849974ee747bf8ed9716b1997075f
Source dataset
uspto-grants-1984_02
Patent number
US04431647

Reaction notes

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