Hydrochloric Acid → HCID 178431792, compound

HRID 1585981Notes

Reaction equation

HRID 1585981 reaction equation
O.[NH2:2][NH2:3].Cl.[CH3:5][C:6]1[C:7]([O:9][C:10](=O)[C:11]=1[CH3:12])=[O:8]>O>[OH:8][C:7]1[N:2]=[N:3][C:10]([OH:9])=[C:11]([CH3:12])[C:6]=1[CH3:5]

Participants

5

Reactant 3

HCID 313Hydrochloric AcidHCID 13010Dimethylmaleic anhydrideHCID 24654Hydrazine hydrate (1:1)

Product 1

HCID 178431792HCID 178431792, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

50 ml of purified water was added to 3.4 ml(0.07 mol) of hydrazine monohydrate and then 14 ml(0.14 mol) of conc. hydrochloric acid was added dropwise thereto. Then, the reaction solution was warmed to boil. When the reaction mixture begins to reflux, 8.83 g(0.07 mol) of 2,3-dimethylmaleic acid anhydride was added thereto. The reaction solution was continuously refluxed for 3 hours and then cooled. The precipitated white crystal was filtered, washed with purified water, dissolved in boiling purified water to remove insoluble material and then recrystallized to obtain the title compound as an amorphous white crystal.

Workup

  1. temperatureThen, the reaction solution was warmed to boil
  2. temperatureto reflux
  3. temperatureThe reaction solution was continuously refluxed for 3 hours
  4. temperaturecooled
  5. filtrationThe precipitated white crystal was filtered
  6. washwashed with purified water
  7. dissolutiondissolved
  8. customin boiling purified water
  9. customto remove insoluble material
  10. customrecrystallized

Sources & evidence

ORD record
ord-5105dc1dcf47497e8d53af88329f8cee
Source dataset
uspto-grants-1999_08
Patent number
US05942511

Reaction notes

Loading…