Reaktionsgleichung
[NH2:1][C:2]1[CH:10]=[CH:9][C:8]([I:11])=[CH:7][C:3]=1[C:4](O)=[O:5].C(O)(=O)C.[O-:16][C:17]#[N:18].[K+].[OH-].[Na+]>O.C1COCC1>[I:11][C:8]1[CH:7]=[C:3]2[C:2](=[CH:10][CH:9]=1)[NH:1][C:17](=[O:16])[NH:18][C:4]2=[O:5]Komponenten
Versuchsvorschrift
To a mixture of 25.36 g of 2-amino-5-iodobenzoic acid in 250 ml of water and 90 mL of THF was added 7.40 g of glacial acetic acid and stirred at room temperature. Then was added 7.82 g of potassium cyanate in water dropwise. Left to overnight. Added another 5.47 g of potassium cyanate. Stirred overnight. A total of 160 g of NaOH pellets were added portionwise, keeping the mixture cool in ice-water bath. The mixture was stirred at room temperature overnight. The mixture was cooled in a refrigerator and the precipitate filtered through a sintered glass funnel. The precipitate was then dissolved in water and acidified with 4N HCl. The precipitate was collected by filtration. The solid was dried in a vacuum oven to yield 25.44 g of the title compound.
Aufarbeitung
- stirringStirred overnight
- stirringThe mixture was stirred at room temperature overnight
- temperatureThe mixture was cooled in a refrigerator
- filtrationthe precipitate filtered through a sintered glass funnel
- dissolutionThe precipitate was then dissolved in water
- filtrationThe precipitate was collected by filtration
- customThe solid was dried in a vacuum oven
Quellen und Nachweise
- ORD-Eintrag
- ord-318027e0e75040bdb499c40da42c5e2a
- Quelldatensatz
- uspto-grants-1995_07
- Patentnummer
- US05436233
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