1,2,3-Triazine synthesis
- Product Name:1,2,3-Triazine
- CAS Number:289-96-3
- Molecular formula:C3H3N3
- Molecular Weight:81.08
288-13-1
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Yield:-
Reaction Conditions:
Stage #1:NH-pyrazole with sodium hydroxide;hydroxylamine-O-sulfonic acid in water at 0; for 0.5 h;
Stage #2: with sodium periodate in dichloromethane;water at 0; for 12 h;
Steps:
General procedure for syntheses of substrates a
General procedure: Solid hydroxylamine-O-sulfonic acid (15.0 mmol, 1.70 g) was slowly added to a solution of pyrazole (5.0 mmol) in 3.7 M NaOH (25.0 mL), then the reaction system was stirred at 0 °C for 0.5 h. After that, the reaction mixture was extracted three times with CH2Cl2. The combined organic layer was washed with saturated brine, dried over with anhydrous Na2SO4 and concentrated in vacuo.The crude product was dissolved in a mixed solution of CH2Cl2 (20.0 mL)/H2O (6.7mL), then NaIO4 (10.0 mmol, 2.14 g) was slowly added and the reaction system was stirred at 0 °C for 12.0 h. After that, the reaction system was warmed to room temperature. The reaction mixture was extracted three times with CH2Cl2, the combined organic layer was washed with saturated brine, dried over with anhydrous Na2SO4 and concentrated in vacuo. The crude residue was purified through column chromatography on silica gel with PE/EA as the eluent to afford the desired substrate.
References:
Zhang, Yuan;Luo, Han;Lu, Qixing;An, Qiaoyu;Li, You;Li, Shanshan;Tang, Zongyuan;Li, Baosheng [Chinese Chemical Letters,2021,vol. 32,# 1,p. 393 - 396] Location in patent:supporting information
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