Hydrochloric Acid → HCID 178526838, compound

HRID 601481

Reaction equation

HRID 601481 reaction equation
Cl.[OH:2][C:3]1[CH:8]=[CH:7][C:6]([N+:9]([O-:11])=[O:10])=[CH:5][N:4]=1.[Cl:12]([O-])(=O)=O.[K+]>O>[Cl:12][C:8]1[C:3]([OH:2])=[N:4][CH:5]=[C:6]([N+:9]([O-:11])=[O:10])[CH:7]=1

Participants

5

Reactant 3

HCID 313Hydrochloric AcidHCID 6426889Potassium ChlorateHCID 178526703HCID 178526703, compound

Product 1

HCID 178526838HCID 178526838, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Conditions

Temperature
53 °C

Procedure

Concentrated hydrochloric acid (239 g) was added to 2-hydroxy-5-nitropyridine (40.0 g). The resulting slurry was heated to 53° C., and stirred until all the solids dissolved. To this was slowly added a solution of potassium chlorate (14.0 g) in water (250 g), while maintaining the temperature between 55° C. and 59° C. The resulting mixture was stirred at 58-62° C. for about 1 hour. The reaction was then cooled to room temperature, stirred for 12 hours and then filtered. After washing the wet cake with water, the product was dried in a vacuum oven. 1H NMR (400 MHz/DMSO-d6) δ 8.64 (d, J=2.9 Hz, 1H), 8.35 (d, J=2.9 Hz, 1H)

Workup

  1. dissolutiondissolved
  2. temperaturewhile maintaining the temperature between 55° C. and 59° C
  3. stirringThe resulting mixture was stirred at 58-62° C. for about 1 hour
  4. temperatureThe reaction was then cooled to room temperature
  5. stirringstirred for 12 hours
  6. filtrationfiltered
  7. washAfter washing the wet cake with water
  8. customthe product was dried in a vacuum oven

Sources & evidence

ORD record
ord-492c546b2d804bae9106948c18fa0755
Source dataset
uspto-grants-2011_03
Patent number
US07902371B2

Linked notes

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