Hydrochloric Acid → HCID 178526838, compound
Reaction equation
[OH:1][C:2]1[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[CH:4][N:3]=1.[ClH:11]>O>[Cl:11][C:7]1[C:2]([OH:1])=[N:3][CH:4]=[C:5]([N+:8]([O-:10])=[O:9])[CH:6]=1Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Conditions
- Temperature
- 0 °C
Procedure
To a warm (50° C.) solution of 2-hydroxy-5-nitro-pyridine (17 g, 121 mmol) in concentrated HCl (80 mL) was added dropwise NaClO3 (4.5 g, 42.5 mmol) in water (70 mL), keeping the internal temperature below 60° C. The reaction mixture was stirred for 15 min and then cooled to 0° C. The resulting precipitate was collected by vacuum filtration and dried to provide 19.7 g of the title compound. ESI-MS: 173 [M−H]− (LC-MS 2); Rf=0.55 (hexane/EtOAc, 1:1).
Workup
- customthe internal temperature below 60° C
- filtrationThe resulting precipitate was collected by vacuum filtration
- customdried
Sources & evidence
- ORD record
- ord-b9259b197ff8475398604bcd4a75a526
- Source dataset
- uspto-grants-2014_08
- Patent number
- US08815926B2
Reaction notes
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