Sodium Acetate → HCID 20222624, compound

HRID 979739Notes

Reaction equation

HRID 979739 reaction equation
[CH2:1]([N:8]1[CH2:11][CH:10]([CH2:12]Cl)[CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[C:14]([O-:17])(=[O:16])[CH3:15].[Na+]>CN(C)C=O>[CH2:1]([N:8]1[CH2:11][CH:10]([CH2:12][O:17][C:14](=[O:16])[CH3:15])[CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

Participants

4

Reactant 2

HCID 517045Sodium AcetateHCID 20222625HCID 20222625, compound

Product 1

HCID 20222624HCID 20222624, compound

Reagents, catalysts & solvents 1

HCID 6228DimethylformamideSolvent

Procedure

195.5 g of 1 was added, drop-by-drop over 45 minutes, to a stirred mixture of 164 g of anhydrous sodium acetate and 1.8 liters of dimethylformamide, at 130° C. The mixture was held at 130° C. for an additional 2.25 hours, then most of the solvent was evaporated under reduced pressure and the cooled residue and treated with sufficient of an ice/water mixture to dissolve the salts therein. The resulting mixture was extracted with ether, the extract was washed with water, and the solvent was evaporated to give 2, as a pale yellow oil, b.p.: 94° C., 0.1 Torr.

Workup

  1. custommost of the solvent was evaporated under reduced pressure
  2. additionthe cooled residue and treated with sufficient of an ice/water mixture
  3. dissolutionto dissolve the salts
  4. extractionThe resulting mixture was extracted with ether
  5. washthe extract was washed with water
  6. customthe solvent was evaporated
  7. customto give 2

Sources & evidence

ORD record
ord-ba2791ea1c5d462db982563550fa8af1
Source dataset
uspto-grants-1987_01
Patent number
US04634554

Reaction notes

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