Hydrochloric Acid → HCID 178433053, compound
Reaction equation
[I:1][C:2]1[NH:6][C:5]([C:7]([O:9]CC)=[O:8])=[N:4][C:3]=1[CH3:12].[OH-].[Na+].Cl>CO.O>[I:1][C:2]1[NH:6][C:5]([C:7]([OH:9])=[O:8])=[N:4][C:3]=1[CH3:12]Participants
6
Reactant 3
Product 1
Reagents, catalysts & solvents 2
Conditions
- Temperature
- 60 °C
Procedure
Into a 100-mL round-bottom flask, was placed a solution of ethyl 5-iodo-4-methyl-1H-imidazole-2-carboxylate (compound 239.2, 200 mg, 0.71 mmol) in methanol (4 mL). A solution of sodium hydroxide (114 mg, 2.85 mmol) in water (2 mL) was added to the reaction. The reaction mixture was stirred for 2 h at 60° C. The pH of the solution was adjusted to 1-2 with hydrogen chloride (1 M). The resulting mixture was concentrated under reduced pressure. Methanol (5 mL) was added to the residue. The salt was filtered off and the filtrate was concentrated under reduced pressure to give 290 mg (crude) of the title compound as a white solid.
Workup
- customInto a 100-mL round-bottom flask, was placed
- concentrationThe resulting mixture was concentrated under reduced pressure
- additionMethanol (5 mL) was added to the residue
- filtrationThe salt was filtered off
- concentrationthe filtrate was concentrated under reduced pressure
Sources & evidence
- ORD record
- ord-d55a9e9b3f694d9c9f950837a8cb12ca
- Source dataset
- uspto-grants-2016_08
- Patent number
- US09428502B2
Reaction notes
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