Reaction equation
[NH2:1][C:2]1[CH:11]=[CH:10][C:5]([C:6]([O:8]C)=[O:7])=[CH:4][C:3]=1[NH:12][C:13]([C:15]1[C:16](=[O:27])[NH:17][N:18]=[C:19]([C:21]2[CH:26]=[CH:25][N:24]=[CH:23][CH:22]=2)[CH:20]=1)=O.O1CCCC1.[OH-].[Li+].Cl>O.CO>[O:27]=[C:16]1[C:15]([C:13]2[NH:1][C:2]3[CH:11]=[CH:10][C:5]([C:6]([OH:8])=[O:7])=[CH:4][C:3]=3[N:12]=2)=[CH:20][C:19]([C:21]2[CH:26]=[CH:25][N:24]=[CH:23][CH:22]=2)=[N:18][NH:17]1Participants
7
Reactant 4
Product 1
Reagents, catalysts & solvents 2
Conditions
- Temperature
- 50 °C
Procedure
A mixture consisting of 500 mg of methyl 4-amino-3-[(3-oxo-6-pyridin-4-yl-2,3-dihydropyridazine-4-carbonyl)amino]benzoate, 6 ml of tetrahydrofuran (THF), 6 ml of methanol, 6 ml of water and 173 mg of lithium hydroxide is stirred at 50° C. for 5 hours. After cooling to room temperature, the pH is adjusted to 4-5 with 1N HCl, whereupon a precipitate separates out and is filtered off with suction and then washed with water and dried in vacuo.
Workup
- temperatureAfter cooling to room temperature
- filtrationis filtered off with suction
- washwashed with water
- customdried in vacuo
Sources & evidence
- ORD record
- ord-c9bb08cc1d4b47fe82080c0420ddf671
- Source dataset
- uspto-grants-2010_07
- Patent number
- US07754713B2
Linked notes
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