Acetone → HCID 22314812, compound

HRID 478589Notes

Reaction equation

HRID 478589 reaction equation
CC(C)=O.[O-]S([O-])(=O)=O.[Mg+2].[CH2:11]([N:18]1[CH2:23][CH2:22][NH:21][CH2:20][CH2:19]1)[C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1.O[C:25]([CH3:29])([CH3:28])[C:26]#[N:27]>CN(C)C(=O)C>[CH2:11]([N:18]1[CH2:23][CH2:22][N:21]([C:25]([CH3:29])([CH3:28])[C:26]#[N:27])[CH2:20][CH2:19]1)[C:12]1[CH:13]=[CH:14][CH:15]=[CH:16][CH:17]=1

Participants

6

Reactant 4

HCID 180AcetoneHCID 6406Acetone CyanohydrinHCID 24083Sulfuric acid magnesium salt (1:1)HCID 759941-Benzylpiperazine

Product 1

HCID 22314812HCID 22314812, compound

Reagents, catalysts & solvents 1

HCID 31374DimethylacetamideSolvent

Conditions

Temperature
45 °C

Procedure

4.5 ml of acetone, 20 g of dry MgSO4, 10 g of N,N-dimethylacetamide, 10 g of 1-benzylpiperazine and 9.5 ml of 2-hydroxyisobutyronitrile are mixed together and heated at 45° C. for 48 hours with vigorous stirring. The reaction mixture is poured onto ice and left stirring for 30 minutes. The mixture is extracted with ether, the organic phase is washed several times with water and dried over Na2SO4, and the solvent is evaporated off under vacuum. 13 g of the expected product are obtained.

Workup

  1. additionThe reaction mixture is poured onto ice
  2. waitleft
  3. extractionThe mixture is extracted with ether
  4. washthe organic phase is washed several times with water
  5. dry with materialdried over Na2SO4
  6. customthe solvent is evaporated off under vacuum

Sources & evidence

ORD record
ord-47dd503360ee4b85a53873c7e5d8a5a3
Source dataset
uspto-grants-2003_11
Patent number
US06642233B1

Reaction notes

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