Ammonia → HCID 178430719, compound
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]=1Participants
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
- additionis progressively added
- customthe precipitate obtained
- customis collected on a filter
- washwashed with water
- customdried
- 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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