Reaction equation
[C:1]1([CH2:7][S:8][C:9]2[N:14]=[C:13]([OH:15])[CH:12]=[C:11]([OH:16])[N:10]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[N+:17]([O-])([OH:19])=[O:18]>C(O)(=O)C>[N+:17]([C:12]1[C:13]([OH:15])=[N:14][C:9]([S:8][CH2:7][C:1]2[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=2)=[N:10][C:11]=1[OH:16])([O-:19])=[O:18]Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Conditions
- Temperature
- 50 °C
Procedure
The product of example 2, step (a) (2 g) was added to a mixture of glacial acetic acid (50 ml) and concentrated nitric acid (20 ml) and the reaction mixture heated to 50° C. A further 28 g of the product of step (a) was added in portions over 2 hours whilst maintaining the reaction temperature between 50 and 60° C. After stirring the reaction mixture for a further 1 hour at 50° C. it was poured onto crushed ice and the subtitled product isolated by filtration as a yellow solid (12.3 g).
Workup
- temperaturewhilst maintaining the reaction temperature between 50 and 60° C
- additionwas poured
- customonto crushed ice
Sources & evidence
- ORD record
- ord-ffafc2ae86d3404bb5bea23cc031402e
- Source dataset
- uspto-grants-2005_10
- Patent number
- US06958344B2
Linked notes
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