Hydrazine hydrate (1:1) → HCID 13385671, compound

HRID 464254Notes

Reaction equation

HRID 464254 reaction equation
Cl[C:2]1[C:11]([O:12][CH3:13])=[N:10][C:9]2[C:4](=[CH:5][CH:6]=[C:7]([F:14])[CH:8]=2)[N:3]=1.O.[NH2:16][NH2:17]>C(O)C>[F:14][C:7]1[CH:8]=[C:9]2[C:4](=[CH:5][CH:6]=1)[N:3]=[C:2]([NH:16][NH2:17])[C:11]([O:12][CH3:13])=[N:10]2

Participants

4

Reactant 2

HCID 24654Hydrazine hydrate (1:1)2×HCID 13385670HCID 13385670, compound

Product 1

HCID 13385671HCID 13385671, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Conditions

Temperature
20 °C

Procedure

To a solution consisting of 47 g. (0.22 mole) of 2-chloro-6-fluoro-3-methoxyquinoxaline dissolved in 1000 ml. of ethanol, there were added 27.6 g. (0.55 mole) of hydrazine hydrate (26.8 ml.). The resulting mixture was stirred at room temperature overnight (i.e., at ca. 20° C. for approximately 16 hours). An additional amount of hydrazine hydrate (9.0 ml.) was then added and the final reaction mixture was allowed to stir at room temperature for a period of four hours. At this point, the precipitate was filtered and washed with ethanol to ultimately afford 43.3 g. (94%) of pure 6-fluoro-2-hydrazino-3-methoxyquinoxaline, m.p. 170°-174° C. (decomp.).

Workup

  1. customthe final reaction mixture
  2. stirringto stir at room temperature for a period of four hours
  3. filtrationAt this point, the precipitate was filtered
  4. washwashed with ethanol to ultimately afford 43.3 g

Sources & evidence

ORD record
ord-bf7e81acdcd54657adf08fde6bb28931
Source dataset
uspto-grants-1985_10
Patent number
US04547501

Reaction notes

Loading…