Sodium Sulfate → HCID 54212115, compound

HRID 262738Notes

Reaction equation

HRID 262738 reaction equation
[CH:1]1([C:4]([N:6]2[CH2:25][CH2:24][C@@:13]34[C:14]5[CH:15]=[C:16]([O:21][CH2:22][CH3:23])[CH:17]=[CH:18][C:19]=5[CH2:20][C@@H:7]2[C@@H:8]3[CH2:9][CH2:10][O:11][CH2:12]4)=O)[CH2:3][CH2:2]1.[H-].[Al+3].[Li+].[H-].[H-].[H-].S([O-])([O-])(=O)=O.[Na+].[Na+]>O1CCCC1.[OH-].[Na+]>[CH:1]1([CH2:4][N:6]2[CH2:25][CH2:24][C@@:13]34[C:14]5[CH:15]=[C:16]([O:21][CH2:22][CH3:23])[CH:17]=[CH:18][C:19]=5[CH2:20][C@@H:7]2[C@@H:8]3[CH2:9][CH2:10][O:11][CH2:12]4)[CH2:2][CH2:3]1

Participants

6

Reactant 3

HCID 24436Sodium Sulfate2×HCID 21226445Aluminium lithium hydrideHCID 54549235HCID 54549235, compound

Product 1

HCID 54212115HCID 54212115, compound

Reagents, catalysts & solvents 2

HCID 14798Sodium HydroxideCatalystHCID 8028TetrahydrofuranSolvent2×

Procedure

The product of Step (c) (XXXIII) (0.005 m) in tetrahydrofuran (20 ml) is added to a suspension of lithium aluminum hydride (0.57 g) in tetrahydrofuran (20 ml), and the mixture is heated at reflux for 18 hours. The mixture is then cooled and saturated sodium sulfate solution (1.8 ml) and a few drops of dilute sodium hydroxide are cautiously added. The mixture is warmed until the solids are completely white. Solid sodium sulfate is added, the solids are removed by filtration and washed well with ethyl acetate. Concentration of the combined filtrate and washes gives the title product.

Workup

  1. temperaturethe mixture is heated
  2. temperatureat reflux for 18 hours
  3. temperatureThe mixture is then cooled
  4. temperatureThe mixture is warmed until the solids
  5. customthe solids are removed by filtration
  6. washwashed well with ethyl acetate

Sources & evidence

ORD record
ord-13ae048076e64b29878e0f0057756d92
Source dataset
uspto-grants-1979_05
Patent number
US04154932

Reaction notes

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