Ammonia → HCID 14231090, compound

HRID 579743Notes

Reaction equation

HRID 579743 reaction equation
P(Cl)(Cl)([Cl:3])=O.[CH3:6][O:7][CH:8]1[C:12]2[N:13]=[CH:14][NH:15][C:16](=O)[C:11]=2[CH2:10][CH2:9]1.N>C(Cl)(Cl)Cl>[Cl:3][C:16]1[C:11]2[CH2:10][CH2:9][CH:8]([O:7][CH3:6])[C:12]=2[N:13]=[CH:14][N:15]=1

Participants

5

Reactant 3

HCID 222AmmoniaHCID 24813Phosphorus oxychlorideHCID 135583111HCID 135583111, compound

Product 1

HCID 14231090HCID 14231090, compound

Reagents, catalysts & solvents 1

HCID 6212ChloroformSolvent

Procedure

2.5 ml of phosphorus oxychloride were added to 1.0 g of 6,7-dihydro-7-methoxy-3H,5H-cyclopenta[d]pyrimidin-4-one [prepared as described in step (d) above], and the mixture was heated under reflux for 5 minutes. The mixture was then cooled to room temperature, 20 ml of chloroform were added, and the mixture was then poured into ice-water. The cold mixture was made alkaline by the addition of concentrated aqueous ammonia, and then the chloroform layer was separated. This chloroform layer was washed with water, dried over anhydrous sodium sulfate and treated with active carbon. The chloroform was then evaporated off under reduced pressure, to give 1.01 g of the title compound as a colorless oil.

Workup

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 5 minutes
  3. customthe chloroform layer was separated
  4. washThis chloroform layer was washed with water
  5. dry with materialdried over anhydrous sodium sulfate
  6. additiontreated with active carbon
  7. customThe chloroform was then evaporated off under reduced pressure

Sources & evidence

ORD record
ord-959e895aa6f54b9ba5b8cc38cb4cb3a6
Source dataset
uspto-grants-1988_06
Patent number
US04749704

Reaction notes

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