Acetic Anhydride → HCID 24839015, compound

HRID 249338Notes

Reaction equation

HRID 249338 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

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-25d2c5e2f6f84716a484b1fe04e4b3ca
Source dataset
uspto-grants-1993_05
Patent number
US05214063

Reaction notes

Loading…