Reaktionsgleichung
Cl.[NH2:2][OH:3].[OH-].[Na+].[Cl:6][C:7]1[CH:8]=[C:9]([OH:17])[C:10](=[CH:15][CH:16]=1)[C:11](OC)=[O:12].N#N>O1CCOCC1.O>[Cl:6][C:7]1[CH:16]=[CH:15][C:10]([C:11]([NH:2][OH:3])=[O:12])=[C:9]([OH:17])[CH:8]=1Komponenten
Versuchsvorschrift
Hydroxylamine hydrochloride in solid (5.25 g, 75 mmol) is placed in an egg type flask and dissolved by drop-adding small amount of water in ice-bath. Thereafter, thereto is drop-added 15 ml of 50% NaOH solution. The reaction is stirred for 5 minutes and is drop-added 50 ml of dioxane solution of methyl 4-chloro-salicylate (9.3 g, 50 mmol) under coverage of N2. After completion of drop-addition, a reaction is carried out at room temperature for 24 hours, and then a red-brown deposit precipitates, which is filtered out and placed in an egg type flask, thereto is added 50 ml of 10% hydrochloric acid and then reflux for 0.5 hour. After cooling to room temperature, a yellow deposit precipitates, which is filtered out and recrystallized in anhydrous ethanol, to obtain 8.25 g of 4-chloro-N,2-dihydroxy-benzamide, with a yield of 88%.
Aufarbeitung
- dissolutiondissolved
- additionAfter completion of drop-addition
- waita reaction is carried out at room temperature for 24 hours
- customa red-brown deposit precipitates
- filtrationwhich is filtered out
- customplaced in an egg type flask
- additionis added 50 ml of 10% hydrochloric acid
- temperaturereflux for 0.5 hour
- customa yellow deposit precipitates
- filtrationwhich is filtered out
- customrecrystallized in anhydrous ethanol
Quellen und Nachweise
- ORD-Eintrag
- ord-3dc1ff1953f34910b1c537f59d973b46
- Quelldatensatz
- uspto-grants-2014_02
- Patentnummer
- US08653069B2
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