Phosphorus oxybromide → HCID 19381666, compound

HRID 2209869Notes

Reaction equation

HRID 2209869 reaction equation
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]2[N:10]=[CH:11][C:12](=O)[NH:13][CH:14]=2)=[CH:5][CH:4]=1.P(Br)(Br)([Br:18])=O>O>[Br:18][C:12]1[CH:11]=[N:10][C:9]([C:6]2[CH:7]=[CH:8][C:3]([O:2][CH3:1])=[CH:4][CH:5]=2)=[CH:14][N:13]=1

Participants

4

Reactant 2

HCID 24613Phosphorus oxybromideHCID 126714395-(4-Methoxyphenyl)pyrazin-2(1H)-one

Product 1

HCID 19381666HCID 19381666, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

26.1 g of 5-(4-methoxyphenyl)-2(1H)pyrazinone and 140 g of phosphorusoxybromide are heated to 100° C. for 45 minutes. After cooling, the hardened mass is added in batches to ice and water, with stirring. After 30 minutes stirring the mixture is left to stand for 18 hours and the precipitate is suction filtered. The filtrate is extracted with methylene chloride and the precipitate is dissolved in methylene chloride extract. The methylene chloride solution is washed with sodium bicarbonate solution, dried, filtered over activated charcoal and evaporated down.

Workup

  1. temperatureAfter cooling
  2. stirringAfter 30 minutes stirring the mixture
  3. waitis left
  4. filtrationfiltered
  5. extractionThe filtrate is extracted with methylene chloride
  6. dissolutionthe precipitate is dissolved in methylene chloride
  7. extractionextract
  8. washThe methylene chloride solution is washed with sodium bicarbonate solution
  9. customdried
  10. filtrationfiltered over activated charcoal
  11. customevaporated down

Sources & evidence

ORD record
ord-274063bdc9ee490884458502300f3089
Source dataset
uspto-grants-1995_10
Patent number
US05455348

Reaction notes

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