Hydrochloric Acid → HCID 178526838, compound

HRID 869059Notes

Reaction equation

HRID 869059 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]=1

Participants

4

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. tR: 5.45 min (HPLC 3); ESI-MS: 173 [M−H]− (LC-MS 2); Rf=0.55 (hexane/EtOAc, 1:1).

Workup

  1. customthe internal temperature below 60° C
  2. filtrationThe resulting precipitate was collected by vacuum filtration
  3. customdried

Sources & evidence

ORD record
ord-918cae79b1c54caf914e03143301dcce
Source dataset
uspto-grants-2015_03
Patent number
US08969341B2

Reaction notes

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