Hydrochloric Acid → HCID 178437926, compound

HRID 1731919Notes

Reaction equation

HRID 1731919 reaction equation
C[O:2][C:3]1[C:4]2[N:5]([C:15]([CH2:18][CH3:19])=[N:16][N:17]=2)[C:6]2[C:11]([N:12]=1)=[CH:10][C:9]([O:13][CH3:14])=[CH:8][CH:7]=2.Cl>C(O)(=O)C>[CH2:18]([C:15]1[N:5]2[C:6]3[C:11]([N:12]=[C:3]([OH:2])[C:4]2=[N:17][N:16]=1)=[CH:10][C:9]([O:13][CH3:14])=[CH:8][CH:7]=3)[CH3:19]

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 133856951-Ethyl-4,7-dimethoxy-[1,2,4]triazolo[4,3-a]quinoxaline

Product 1

HCID 178437926HCID 178437926, compound

Reagents, catalysts & solvents 1

HCID 176Acetic AcidSolvent

Procedure

A mixture consisting of 3.3 g. (0.013 mole) of 4,7-dimethoxy-1-ethyl-[1,2,4]triazolo[4,3-a]quinoxaline, 33 ml. of 1N hydrochloric acid and 99 ml. of glacial acetic acid was refluxed for a period of two hours. Upon completion of this step, the reaction mixture was cooled to room temperature and poured over ice/water. The resulting mixture was then stirred for a period of 20 minutes and extracted with ethyl acetate. The latter extract next washed with saturated brine and dried over anhydrous magnesium sulfate. After removal of the drying agent by means of filtration and the solvent by means of evaporation under reduced pressure, there was finally obtained a yellowish solid product which was washed with water and air-dried to constant weight to ultimately afford 1.87 g. (67%) of pure 1-ethyl-4-hydroxy-7-methoxy[1,2,4]triazolo[4,3-a]quinoxaline, m.p. >250° C.

Workup

  1. extractionextracted with ethyl acetate
  2. extractionThe latter extract next
  3. washwashed with saturated brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. customAfter removal of the drying agent
  6. filtrationby means of filtration
  7. customthe solvent by means of evaporation under reduced pressure, there
  8. customwas finally obtained a yellowish solid product which
  9. washwas washed with water
  10. customair-dried to constant weight to ultimately afford 1.87 g

Sources & evidence

ORD record
ord-861c162be2a44c40969d6a37ce83236d
Source dataset
uspto-grants-1986_11
Patent number
US04623725

Reaction notes

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