Potassium Carbonate → HCID 15003628, compound

HRID 373452Notes

Reaction equation

HRID 373452 reaction equation
[Cl:1][C:2]1[C:7]([O:8][CH3:9])=[C:6](Cl)[N:5]=[C:4]([S:11][CH3:12])[N:3]=1.C(=O)([O-])[O-].[K+].[K+].O.[NH2:20][NH2:21]>O>[Cl:1][C:2]1[C:7]([O:8][CH3:9])=[C:6]([NH:20][NH2:21])[N:5]=[C:4]([S:11][CH3:12])[N:3]=1

Participants

5

Reactant 3

HCID 11430Potassium CarbonateHCID 24654Hydrazine hydrate (1:1)HCID 15003627HCID 15003627, compound

Product 1

HCID 15003628HCID 15003628, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

A mixture of 48.1 g (0.21 mol) of 4,6-di-chloro-2-methylthio-5-methoxypyrimidine, 29.5 g (0.21 mol) of potassium carbonate, 80 ml of hydrazine monohydrate, and 80 ml of water was prepared and heated at reflux with stirring for about 30 min at which time the reaction appeared by high pressure liquid chromatography to be complete. The mixture was allowed to cool and was extracted with methylene chloride. The extract was dried over magnesium sulfate and concentrated under reduced pressure. The residue was mixed with hexane and the solids removed by filtration and dried to obtain 34.7 g of the title compound as a tan solid melting at 118°-119° C.

Workup

  1. customwas prepared
  2. temperatureheated
  3. temperatureat reflux
  4. temperatureto cool
  5. extractionwas extracted with methylene chloride
  6. dry with materialThe extract was dried over magnesium sulfate
  7. concentrationconcentrated under reduced pressure
  8. additionThe residue was mixed with hexane
  9. customthe solids removed by filtration
  10. customdried

Sources & evidence

ORD record
ord-ddde6afe32b24713956b03cef67ff780
Source dataset
uspto-grants-1992_11
Patent number
US05163995

Reaction notes

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