Acetic Anhydride → HCID 24839015, compound

HRID 1197787Notes

Reaction equation

HRID 1197787 reaction equation
[CH3:1][O:2][C:3](=[O:13])[CH2:4][CH:5]([C:8]1[NH:9][CH:10]=[CH:11][N:12]=1)[CH2:6][NH2:7].[C:14](OC(=O)C)(=[O:16])[CH3:15].C(=O)([O-])[O-].[Na+].[Na+]>C(Cl)(Cl)Cl>[CH3:1][O:2][C:3](=[O:13])[CH2:4][CH:5]([C:8]1[NH:9][CH:10]=[CH:11][N:12]=1)[CH2:6][NH:7][C:14](=[O:16])[CH3:15]

Participants

5

Reactant 3

HCID 7918Acetic AnhydrideHCID 10340Sodium CarbonateHCID 24839018HCID 24839018, compound

Product 1

HCID 24839015HCID 24839015, compound

Reagents, catalysts & solvents 1

HCID 6212ChloroformSolvent

Procedure

0.01 mol of the compound obtained in stage B of Example 16 is dissolved in 50 cm3 of chloroform. 0.01 mol of acetic anhydride and 0.015 mol of sodium carbonate are added. The whole is heated under reflux for five hours while stirring. The reaction mixture is then cooled, evaporated to dryness and extracted with chloroform twice. The chloroform phases are combined and dried over calcium chloride and the solvent is evaporated in vacuo on a water bath. The residue is purified by chromatography.

Workup

  1. temperatureThe whole is heated
  2. temperatureunder reflux for five hours
  3. temperatureThe reaction mixture is then cooled
  4. customevaporated to dryness
  5. extractionextracted with chloroform twice
  6. dry with materialdried over calcium chloride
  7. customthe solvent is evaporated in vacuo on a water bath
  8. customThe residue is purified by chromatography

Sources & evidence

ORD record
ord-125129b3bfd345e89bc626477b734039
Source dataset
uspto-grants-1994_01
Patent number
US05278166

Reaction notes

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