Water → HCID 15376210, compound

HRID 2210979Notes

Reaction equation

HRID 2210979 reaction equation
[Cl:1][C:2]1[C:3](OC)=[N:4][C:5]([O:8][CH3:9])=[N:6][CH:7]=1.O.[NH2:13][NH2:14].O>CO>[Cl:1][C:2]1[C:3]([NH:13][NH2:14])=[N:4][C:5]([O:8][CH3:9])=[N:6][CH:7]=1

Participants

5

Reactant 3

HCID 962WaterHCID 24654Hydrazine hydrate (1:1)HCID 142700285-Chloro-2,4-dimethoxypyrimidine

Product 1

HCID 15376210HCID 15376210, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

A solution containing 0.35 g (2.0 mmol) of 5-chloro-2,4-dimethoxypyrimidine and 0.35 g (7.0 mmol) of hydrazine hydrate in 2.9 g of methanol was heated at reflux with stirring for 8 hours. The mixture was then cooled causing a precipitate to form. Water was added until the precipitation appeared to be complete and the precipitate was then recovered by vacuum filtration and allowed to air dry overnight to obtain 0.23 g (66 percent of theory) of the title compound as a white solid. The product melted at 172°-173° C. after changing crystalline form from needles to cube-like shapes in a phenomenon that appeared to involve sublimation.

Workup

  1. temperaturewas heated
  2. temperatureat reflux
  3. temperatureThe mixture was then cooled
  4. customto form
  5. filtrationthe precipitate was then recovered by vacuum filtration
  6. customto air dry overnight

Sources & evidence

ORD record
ord-5ac8dd7e95f544bbbb14f2c9db3c1f1a
Source dataset
uspto-grants-1995_10
Patent number
US05461153

Reaction notes

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