Ammonium Hydroxide → HCID 21432968, compound
Reaction equation
[OH-].[NH4+:2].C[O:4][C:5]([C:7]1[CH:12]=[C:11]([Br:13])[C:10]([OH:14])=[C:9]([Br:15])[N:8]=1)=O>>[Br:13][C:11]1[C:10]([OH:14])=[C:9]([Br:15])[N:8]=[C:7]([C:5]([NH2:2])=[O:4])[CH:12]=1Participants
3
Procedure
Concentrated ammonium hydroxide, 180 ml, was added to 10 g of 4,6-dibromo-5-hydroxy-2-pyridinecarboxylic acid methyl ester and heated at 45°-60° C. for 1 hour. After the mixture was kept for 2 days at room temperature, the solid was filtered and successively washed with dilute HCl (to neutralize the ammonia) and then with methanol and benzene to remove any unreacted starting material. The product was isolated in 80% yield; m.p. 261-266° C. (best sample: m.p. 275° C.).
Workup
- temperatureheated at 45°-60° C. for 1 hour
- filtrationthe solid was filtered
- washsuccessively washed with dilute HCl (
- customto remove
- customThe product was isolated in 80% yield
Sources & evidence
- ORD record
- ord-2500c11cac2b4ba094224738a5d04dfc
- Source dataset
- uspto-grants-1977_05
- Patent number
- US04025333
Reaction notes
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