Sodium Sulfate → HCID 67119693, compound

HRID 387233Notes

Reaction equation

HRID 387233 reaction equation
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]2[CH2:13][NH:12][C:11](=O)[CH2:10][S:9]2)=[CH:4][CH:3]=1.[H-].[Al+3].[Li+].[H-].[H-].[H-].[O-]S([O-])(=O)=O.[Na+].[Na+]>O1CCCC1>[NH2:1][C:2]1[CH:3]=[CH:4][C:5]([CH:8]2[CH2:13][NH:12][CH2:11][CH2:10][S:9]2)=[CH:6][CH:7]=1

Participants

5

Reactant 3

HCID 24436Sodium SulfateHCID 21226445Aluminium lithium hydrideHCID 67119615HCID 67119615, compound

Product 1

HCID 67119693HCID 67119693, compound

Reagents, catalysts & solvents 1

HCID 8028TetrahydrofuranSolvent

Conditions

Temperature
60 °C

Procedure

To the solution of 6-(4-aminophenyl)-thiomorpholin-3-one (0.26 g, 1.25 mmol) in anhydrous tetrahydrofuran (6.7 mL) was added lithium aluminium hydride (0.16 g, 4.27 mmol) in several portions and the mixture was stirred at 60° C. for 2 h. Na2SO4×10H2O (2.00 g) was added in small portions until the complex was decomposed. The suspension was filtered, the solids were washed with tetrahydrofuran (2×3 mL) and the combined filtrates were evaporated. The title compound was obtained as a viscous oil (0.25 g, 1.26 mmol, 100%). ESMS m/z 195 (M+H)+.

Workup

  1. filtrationThe suspension was filtered
  2. washthe solids were washed with tetrahydrofuran (2×3 mL)
  3. customthe combined filtrates were evaporated

Sources & evidence

ORD record
ord-f10d7f15eb814f55a12437dcbca7465f
Source dataset
uspto-grants-2013_02
Patent number
US08372970B2

Reaction notes

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