1-hydroxy-6-nitrobenzotriazole synthesis
- Product Name:1-hydroxy-6-nitrobenzotriazole
- CAS Number:26185-63-7
- Molecular formula:C6H4N4O3
- Molecular Weight:180.12
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Yield: 78%
Reaction Conditions:
with pyridine;sodium acetate;hydrazine hydrate;acetic acid in water at 120; for 24 h;
Steps:
1
Specifically, first Compound 2-3 ( 2,4-Dinitropeneyl hydraz ine, 30 g, 75 mmol, wet with ca. 50% Water ) Pyridine-water It was dissolved in (375 μl, 2: 3, v / v). Hydrazine monohydrate (3.6 ml, 75 mmol), Acetic acid (17.1 ml, 300 mmol), Sodium acetate (21.54 g, 262.5 mmol) was added, and the mixture was heated under reflux for 24 hours. After cooling the reaction solution, diethyl ether and water were added, and the extraction operation was performed three times. The aqueous layer is recovered and the solvent is distilled under reduced pressure. I left. 1M HCl (100 ml) in the obtained crude product Was added and the mixture was stirred at room temperature for 30 minutes. The solid is collected by suction filtration and compound 2-4 (10.5 g, 78%) was obtained.
References:
Tokyo Institute of Technology;Okubo, Akihiro;Ikeda, Kosuke;Miyake, Yu JP2020/132604, 2020, A Location in patent:Paragraph 0094-0095
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