Nitric Acid → HCID 178526845, compound

HRID 1799575Notes

Reaction equation

HRID 1799575 reaction equation
S(=O)(=O)(O)O.[N:6]1[CH:11]=[CH:10][C:9]([OH:12])=[N:8][C:7]=1[OH:13].[N+:14]([O-])([OH:16])=[O:15]>>[N+:14]([C:10]1[C:9]([OH:12])=[N:8][C:7]([OH:13])=[N:6][CH:11]=1)([O-:16])=[O:15]

Participants

4

Conditions

Temperature
0 °C

Procedure

A 3-necked roundbottom flask was charged with sulfuric acid (5400 ml) and the solution was cooled to 0° C. Pyrimidine-2,4-diol (1.0 kg, 8.93 mol) was added in several batches. The resulting solution was allowed to react, with stirring, for 30 minutes. To the above was added nitric acid (1800 ml) dropwise with stirring, while the temperature was maintained at 0° C. The resulting solution was allowed to react, with stirring, for 2 hours. The reaction mixture was then quenched by adding ice water and a precipitate formed. The solid was collected by filtration and dried in an oven under reduced pressure to afford the title compound.

Workup

  1. customto react
  2. stirringwith stirring, while the temperature
  3. temperaturewas maintained at 0° C
  4. customto react
  5. stirringwith stirring, for 2 hours
  6. customThe reaction mixture was then quenched
  7. additionby adding ice water
  8. customa precipitate formed
  9. filtrationThe solid was collected by filtration
  10. customdried in an oven under reduced pressure

Sources & evidence

ORD record
ord-4af49e6be78b46c79d7fdd9f27c61348
Source dataset
uspto-grants-2013_01
Patent number
US08344144B2

Reaction notes

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