Acetic Anhydride → HCID 21704301, compound

HRID 1106419Notes

Reaction equation

HRID 1106419 reaction equation
[NH2:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[N:8]([CH2:12][P:13]([OH:16])(=[O:15])[OH:14])[C:7](=[O:17])[C:6](=[O:18])[NH:5]2.C(=O)([O-])[O-].[Na+].[Na+].[C:25](OC(=O)C)(=[O:27])[CH3:26]>O>[C:25]([NH:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[N:8]([CH2:12][P:13]([OH:16])(=[O:14])[OH:15])[C:7](=[O:17])[C:6](=[O:18])[NH:5]2)(=[O:27])[CH3:26]

Participants

5

Reactant 3

HCID 7918Acetic AnhydrideHCID 10340Sodium CarbonateHCID 21704250HCID 21704250, compound

Product 1

HCID 21704301HCID 21704301, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

100 mg of 1-(6-amino-2,3-dioxo-1,2,3,4-tetrahydroquinoxalin-l-yl)methanephosphonic acid is adjusted in 20 ml of water to a pH of 9.5 with a saturated sodium carbonate solution and combined with 0.2 ml of acetic anhydride. After one hour of stirring, the mixture is concentrated, dissolved in a minimum amount of water, introduced into an ion exchanger (IR 120, strongly acidic), and eluted with water: The corresponding fractions are combined, concentrated, and dried, thus obtaining 110 mg of 1-(6-acetylamino-2,3-dioxo-1,2,3,4-tetrahydroquinoxalin-1-yl)methanephosphonic acid, mp: 120° C.

Workup

  1. concentrationthe mixture is concentrated
  2. dissolutiondissolved in a minimum amount of water
  3. additionintroduced into an ion exchanger (IR 120
  4. washstrongly acidic), and eluted with water
  5. concentrationconcentrated
  6. customdried

Sources & evidence

ORD record
ord-4f525ae901574326b1f059113b5af7a4
Source dataset
uspto-grants-2000_05
Patent number
US06057304

Reaction notes

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