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7-chloro-9H-[1,2,4]triazolo[5,1-b][1,3]benzothiazin-9-one[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
80%
With potassium carbonate; In N,N,N,N,N,N-hexamethylphosphoric triamide; at 80℃; for 24h;Sealed tube; Schlenk technique;
Schlenk reaction tube, <strong>[13421-00-6]5-chloro-2-iodo<strong>[13421-00-6]benzoic acid</strong></strong> (0.5 mmol), 3-mercapto 1,2,4-triazole (0.5 mmol), potassium carbonate (0.1 mmol) and HMPA 2 mL). The reaction tube was sealed and reacted at 80 C for 24 hours under an air atmosphere. After completion of the reaction, acetic acid (1 ml) was added, stirred at room temperature for 1 hour, then extracted twice with methylene chloride. The organic layer was washed three times with saturated brine. The organic layer was dried over anhydrous sodium sulfate and concentrated under reduced pressure. And purified by column chromatography to obtain product 3. The structure and characterization data are as follows
7-nitro-9H-[1,2,4]triazolo[5,1-b][1,3]benzothiazin-9-one[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
71%
With potassium carbonate; In N,N,N,N,N,N-hexamethylphosphoric triamide; at 80℃; for 24h;Sealed tube; Schlenk technique;
Schlenk reaction tube A solution of <strong>[19230-50-3]5-nitro-2-iodobenzoic acid</strong> (0.5 mmol), 3-mercapto 1,2,4-triazole (0.5 mmol), potassium carbonate (0.1 mmol) and HMPA (2 mL). The reaction tube was sealed and reacted at 80 C for 24 hours under an air atmosphere. After completion of the reaction, acetic acid (1 ml) was added, stirred at room temperature for 1 hour, then extracted twice with methylene chloride. The organic layer was washed three times with saturated brine. The organic layer was dried over anhydrous sodium sulfate and concentrated under reduced pressure. And purified by column chromatography to obtain the product 5, and its structure and characterization data are as follows
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