Acetic Acid → HCID 10062631, compound

HRID 48228Notes

Reaction equation

HRID 48228 reaction equation
[NH2:1][C:2]1[C:3]2[CH2:17][CH2:16][N:15]([CH3:18])[CH2:14][C:4]=2[C:5]2[NH:6][C:7](=[O:13])[C:8](=[O:12])[NH:9][C:10]=2[CH:11]=1.[C:19](O)(=[O:21])[CH3:20]>C(OC(=O)C)(=O)C>[CH3:18][N:15]1[CH2:16][CH2:17][C:3]2[C:2]([NH:1][C:19](=[O:21])[CH3:20])=[CH:11][C:10]3[NH:9][C:8](=[O:12])[C:7](=[O:13])[NH:6][C:5]=3[C:4]=2[CH2:14]1

Participants

4

Reactant 2

HCID 176Acetic AcidHCID 99921196-Amino-9-methyl-1,4,7,8,9,10-hexahydro-pyrido[3,4-f]quinoxaline-2,3-dione

Product 1

HCID 10062631HCID 10062631, compound

Reagents, catalysts & solvents 1

HCID 7918Acetic AnhydrideSolvent

Procedure

A mixture of the product from Example 79 (0.27 g, 1.1 mmol) in 25 mL acetic acid and 10 mL acetic anhydride was stirred at room temperature for 18 hours. After removing the solvent, the residue was washed with ether, dissolved in water and then basified with saturated sodium bicarbonate. The flask was cooled in the freezer for 2 hours and the precipitate collected by filtration, washed consecutively with water and ether, and dried over P2O5 in vacuo to give the title compound (0.2 g).

Workup

  1. customAfter removing the solvent
  2. washthe residue was washed with ether
  3. dissolutiondissolved in water
  4. temperatureThe flask was cooled in the freezer for 2 hours
  5. filtrationthe precipitate collected by filtration
  6. washwashed consecutively with water and ether
  7. dry with materialdried over P2O5 in vacuo

Sources & evidence

ORD record
ord-87022b01755e4b0aa47613e8f5c15bb5
Source dataset
uspto-grants-2004_03
Patent number
US06703391B2

Reaction notes

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