Potassium Carbonate → HCID 178496817, compound

HRID 893798Notes

Reaction equation

HRID 893798 reaction equation
CS([C:5]1[N:10]=[C:9]([O:11][CH3:12])[CH:8]=[C:7]([O:13][CH3:14])[N:6]=1)(=O)=O.C(=O)([O-])[O-].[K+].[K+].S(O)(O)(=O)=O.[CH3:26][O:27][C:28](=[NH:30])[NH2:29]>C(#N)C>[CH3:14][O:13][C:7]1[CH:8]=[C:9]([O:11][CH3:12])[N:10]=[C:5]([NH:30][C:28](=[NH:29])[O:27][CH3:26])[N:6]=1

Participants

5

Reactant 3

HCID 11430Potassium CarbonateHCID 169039Carbamimidic acid, methyl ester, sulfate (1:1)HCID 8383634,6-Dimethoxy-2-(methylsulfonyl)pyrimidine

Product 1

HCID 178496817HCID 178496817, compoundYield 171%

Reagents, catalysts & solvents 1

HCID 6342AcetonitrileSolvent

Procedure

54.5 g (0.25 mol) of 2-methylsulphonyl-4,6-dimethoxy-pyrimidine, 69 g (0.5 mol) of potassium carbonate and 1500 ml of acetonitrile are mixed with stirring. 33.85 g (0.1375 mol) of O-methyl-isourea sulphate are then added and the mixture is heated to boiling for 17 hours. After cooling, the solution is filtered off with suction and the mother liquor is concentrated. After taking up the residue in methylene chloride, the solution is washed three times with water, dried and concentrated again. 49.9 g of N-(4,6-dimethoxy-pyrimidin-2-yl)-O-methylisourea are obtained in the form of yellow crystals of melting point 91°-95° C. (90% purity; yield 85% of theory).

Workup

  1. temperaturethe mixture is heated
  2. temperatureAfter cooling
  3. filtrationthe solution is filtered off with suction
  4. concentrationthe mother liquor is concentrated
  5. washthe solution is washed three times with water
  6. customdried
  7. concentrationconcentrated again

Sources & evidence

ORD record
ord-2e112bd10ba34a37969d1bc4e2ca57bd
Source dataset
uspto-grants-1992_06
Patent number
US05126454

Reaction notes

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