Acetic Anhydride → HCID 20248673, compound

HRID 848394Notes

Reaction equation

HRID 848394 reaction equation
S([O-])([O-])=O.[Na+].[Na+].S(O)(O)(=O)=O.[S:12]([NH:16][CH2:17][CH2:18][NH:19][C:20]1[CH:25]=[CH:24][C:23]([NH2:26])=[CH:22][CH:21]=1)([CH3:15])(=[O:14])=[O:13].[C:27](OC(=O)C)(=[O:29])[CH3:28]>O>[C:27]([NH:26][C:23]1[CH:24]=[CH:25][C:20]([NH:19][CH2:18][CH2:17][NH:16][S:12]([CH3:15])(=[O:13])=[O:14])=[CH:21][CH:22]=1)(=[O:29])[CH3:28]

Participants

5

Reactant 3

HCID 7918Acetic AnhydrideHCID 24437Sodium SulfiteHCID 458930N-[2-(4-aminoanilino)ethyl]methanesulfonamide; sulfuric acid

Product 1

HCID 20248673HCID 20248673, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

0.2 mol (25.2 g) of sodium sulphite is added, at ambient temperature, to a solution of 0.1 mol (32.7 g) of N-(β-mesylaminoethyl)-para-phenylenediamine sulphate in 150 ml of water, and 0.13 mol (13.17 g) of acetic anhydride is added gradually, whilst stirring. When the addition is complete, stirring is continued for one hour and the expected acetylated derivative which has precipitated in crystalline form is then filtered off. The product is drained, washed with water and dried in vacuo. After recrystallisation from alcohol and drying in vacuo, it melts at 130° C.

Workup

  1. additionis added gradually
  2. additionWhen the addition
  3. stirringstirring
  4. customthe expected acetylated derivative which has precipitated in crystalline form
  5. filtrationis then filtered off
  6. washwashed with water
  7. customdried in vacuo
  8. customAfter recrystallisation from alcohol
  9. customdrying in vacuo, it melts at 130° C.

Sources & evidence

ORD record
ord-eeefe92c406c44e98bdbe8f2962e95e7
Source dataset
uspto-grants-1981_10
Patent number
US04295848

Reaction notes

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