Sodium Sulfate → HCID 15541828, compound

HRID 279355Notes

Reaction equation

HRID 279355 reaction equation
[H-].[Al+3].[Li+].[H-].[H-].[H-].[C:7]([C:9]1[CH:14]=[CH:13][C:12]([C:15]2[CH2:20][CH2:19][CH:18]([CH:21]([CH3:30])[CH2:22][NH:23][S:24]([CH:27]([CH3:29])[CH3:28])(=[O:26])=[O:25])[CH2:17][CH:16]=2)=[CH:11][CH:10]=1)#[N:8].[O-]S([O-])(=O)=O.[Na+].[Na+]>C(OCC)C.C1COCC1>[NH2:8][CH2:7][C:9]1[CH:14]=[CH:13][C:12]([C:15]2[CH2:20][CH2:19][CH:18]([CH:21]([CH3:30])[CH2:22][NH:23][S:24]([CH:27]([CH3:29])[CH3:28])(=[O:26])=[O:25])[CH2:17][CH:16]=2)=[CH:11][CH:10]=1

Participants

6

Reactant 3

HCID 24436Sodium SulfateHCID 9950130HCID 9950130, compoundHCID 21226445Aluminium lithium hydride

Product 1

HCID 15541828HCID 15541828, compoundYield 64%

Reagents, catalysts & solvents 2

HCID 3283Diethyl EtherSolvent2×HCID 8028TetrahydrofuranSolvent

Procedure

To a suspension of 33 mg (0.87 mmol) of lithium aluminum hydride in 0.5 ml of diethyl ether, 100 mg (0.29 mmol) of the material prepared in Example 14 in 0.5 ml of diethyl ether and 0.5 ml of THF. The mixture was stirred for 3 h. Na2SO4 10H2O was added, and the mixture stirred for 30 min at ambient temperature. The solid was filtered and the organic solution was concentrated in vacuo. Precipitation with diethyl ether afforded 65 mg (64%) of the title compound. Analysis calculated for C19H30N2O2S 0.75H2O: %C, 62.69; %H, 8.72; %N, 7.69. Found: %C, 62.73; %H, 7.96; %N, 7.32. Field Desorption Mass Spectrum: M=350.

Workup

  1. stirringthe mixture stirred for 30 min at ambient temperature
  2. filtrationThe solid was filtered
  3. concentrationthe organic solution was concentrated in vacuo
  4. customPrecipitation with diethyl ether

Sources & evidence

ORD record
ord-18777ec92aba4c10a56588886a71e50f
Source dataset
uspto-grants-2002_03
Patent number
US06362230B1

Reaction notes

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