Sodium Acetate → HCID 88317215, compound

HRID 1939869Notes

Reaction equation

HRID 1939869 reaction equation
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][C:9](=[O:17])[CH2:10][CH:11]([CH3:16])[CH2:12][C:13]([OH:15])=O)=[CH:4][C:3]=1[CH:18]=[C:19]([Cl:25])[C:20]([O:22][CH2:23][CH3:24])=[O:21].C([O-])(=O)C.[Na+]>C(OC(=O)C)(=O)C>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[C:9](=[O:17])[CH2:10][CH:11]([CH3:16])[CH2:12][C:13]2=[O:15])=[CH:4][C:3]=1[CH:18]=[C:19]([Cl:25])[C:20]([O:22][CH2:23][CH3:24])=[O:21]

Participants

4

Reactant 2

HCID 517045Sodium AcetateHCID 86751727HCID 86751727, compound

Product 1

HCID 88317215HCID 88317215, compound

Reagents, catalysts & solvents 1

HCID 7918Acetic AnhydrideSolvent

Procedure

A solution of 2.8 g of N-[4-chloro-3-(2-chloro-2-ethoxycarbonylethenyl)phenyl]-3-methylglutaric acid monoamide and 0.1 g of sodium acetate in 50 ml of acetic anhydride was stirred at 95° C. for 2 h. The solvent was then removed. After dissolving the residue in 150 ml of dichloromethane, it was washed with sodium hydrogen-carbonate solution, water and sodium chloride solution, dried and concentrated in vacuo. The residue which remained was crystallized using petroleum ether, and the crystals were removed and dried. Yield: 2.1 g; m.p.: 82°-84° C.

Workup

  1. customThe solvent was then removed
  2. dissolutionAfter dissolving the residue in 150 ml of dichloromethane
  3. washit was washed with sodium hydrogen-carbonate solution, water and sodium chloride solution
  4. customdried
  5. concentrationconcentrated in vacuo
  6. customThe residue which remained was crystallized
  7. customthe crystals were removed
  8. customdried

Sources & evidence

ORD record
ord-de23c685c0c04b69bc22b44e14c56dca
Source dataset
uspto-grants-1997_12
Patent number
US05698494

Reaction notes

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