Sodium Sulfate → HCID 201858, compound

HRID 1458539Notes

Reaction equation

HRID 1458539 reaction equation
[O:1]1[CH2:6][CH2:5][N:4]([CH2:7][CH:8]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[C:9](OCC)=[O:10])[CH2:3][CH2:2]1.ClCC(C1C=CC=CC=1)C(OCC)=O.[H-].[H-].[H-].[H-].[Li+].[Al+3].S([O-])([O-])(=O)=O.[Na+].[Na+]>CCOCC>[OH:10][CH2:9][CH:8]([C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)[CH2:7][N:4]1[CH2:3][CH2:2][O:1][CH2:6][CH2:5]1

Participants

6

Reactant 4

HCID 24436Sodium SulfateHCID 3794238HCID 3794238, compoundHCID 13948363HCID 13948363, compoundHCID 21226445Aluminium lithium hydride2×

Product 1

HCID 201858HCID 201858, compoundYield 118.8%

Reagents, catalysts & solvents 1

HCID 3283Diethyl EtherSolvent2×

Procedure

Ethyl 3-morpholino-2-phenylpropionate (660 mg, 2.51 mmol) prepared in the above (1) in dry ether (5 ml) was dropwise added to a suspension of LiAlH4 (110 mg, 2.89 mmol) and dry ether (10 ml) while chilling with ice, and then stirred to cause reaction at room temperature for 2 hours. To the resulting solution, saturated aqueous sodium sulfate was added in order to decompose remaining excess LiAlH4. Subsequently, insolubles were removed by filtration. The solvent was removed by distillation under reduced pressure to obtain 660 mg of the titled compound as a colorless oil (yield: 100%)

Workup

  1. temperaturewhile chilling with ice
  2. customreaction at room temperature for 2 hours
  3. customSubsequently, insolubles were removed by filtration
  4. customThe solvent was removed by distillation under reduced pressure

Sources & evidence

ORD record
ord-69fbe3d8c2ff462199133cdf4174c592
Source dataset
uspto-grants-1998_12
Patent number
US05852006

Reaction notes

Loading…