HCID 20562715, compound → HCID 20562713, compound

HRID 1155069Notes

Reaction equation

HRID 1155069 reaction equation
[NH2:1][C:2]1[C:7]([NH:8][C:9](=O)[C:10]2[CH:15]=[CH:14][C:13]([O:16][CH3:17])=[C:12]([O:18][CH3:19])[CH:11]=2)=[CH:6][N:5]=[CH:4][N:3]=1>P(Cl)(Cl)(Cl)=O>[CH3:19][O:18][C:12]1[CH:11]=[C:10]([C:9]2[NH:8][C:7]3[C:2](=[N:3][CH:4]=[N:5][CH:6]=3)[N:1]=2)[CH:15]=[CH:14][C:13]=1[O:16][CH3:17]

Participants

3

Reactant 1

HCID 20562715HCID 20562715, compound

Product 1

HCID 20562713HCID 20562713, compound

Reagents, catalysts & solvents 1

HCID 24813Phosphorus oxychlorideSolvent

Procedure

An amount of 7.5 g of 4-amino-5-(3,4-dimethoxy-benzoylamino)-pyrimidine was refluxed in 100 ml of phosphorus oxychloride for six hours. After evaporation and pouring on water, the solution was neutralized by means of potassium carbonate. The solution was evaporated to dryness, and the residue was extracted with boiling ethanol. The alcoholic solution was evaporated, and the remaining product was purified over silicagel (eluate: methylene chloride/ethanol in a volume ratio of 19:1).

Workup

  1. customAfter evaporation
  2. additionpouring on water
  3. customThe solution was evaporated to dryness
  4. extractionthe residue was extracted with boiling ethanol
  5. customThe alcoholic solution was evaporated
  6. customthe remaining product was purified over silicagel (eluate: methylene chloride/ethanol in a volume ratio of 19:1)

Sources & evidence

ORD record
ord-873696e511574af2aa3eef68d912728a
Source dataset
uspto-grants-1981_11
Patent number
US04299834

Reaction notes

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