Ammonia → HCID 178430719, compound

HRID 2210428Notes

Reaction equation

HRID 2210428 reaction equation
N[C:2]1[CH:7]=[CH:6][C:5]([CH3:8])=[CH:4][N:3]=1.[N+:9]([O-])([OH:11])=[O:10].N.S(=O)(=O)(O)[OH:15]>>[OH:15][C:2]1[C:7]([N+:9]([O-:11])=[O:10])=[CH:6][C:5]([CH3:8])=[CH:4][N:3]=1

Participants

5

Conditions

Temperature
130 °C

Procedure

25 g of 2-amino-5-methylpyridine are dissolved in 50 cm3 of concentrated sulfuric acid in a 600 cm3 round- bottomed flask. A mixture consisting of 40 cm3 of concentrated nitric acid and 40 cm3 of concentrated sulfuric acid is progressively added. The reaction mixture heats up with formation of foam. The temperature is maintained constant at 130° C. throughout the duration of the addition of the acid. The colored solution is then poured onto 300 g of ice and the pH is brought to around 3-4 by addition of aqueous ammonia. After standing in a refrigerator, the precipitate obtained is collected on a filter, washed with water and dried. It is recrystallized from hot water.

Workup

  1. additionis progressively added
  2. customthe precipitate obtained
  3. customis collected on a filter
  4. washwashed with water
  5. customdried
  6. customIt is recrystallized from hot water

Sources & evidence

ORD record
ord-ffc265e545184f82bbd79dd9d9de62b6
Source dataset
uspto-grants-1995_10
Patent number
US05459138

Reaction notes

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