反应详情

温度

100 °C

A reaction vessel was charged with DMF (1.225 L), Preparation 21, 4-iodo-1-methyl-1H-pyrazole-5-carbonitrile (175 g, 751 mmol), sodium azide (147 g, 2.25 mol), and ammonium chloride (121 g, 2.25 mol). H2O (525 mL) was added slowly to minimize exotherm. The reaction mixture was heated at 100° C. overnight. The reaction mixture was cooled to room temperature and poured into a mixture of H2O (2 L) and ice (1 kg). An aqueous solution of NaNO2 (600 mL, 120 g NaNO2, 20% by weight) was added followed by the slow addition of aqueous H2SO4 until the pH of the reaction mixture was 1. The precipitate was collected via filtration, washed with H2O and dried in vacuo to afford 5-(4-iodo-1-methyl-1H-pyrazol-5-yl)-2H-tetrazole as a colorless solid (187 g, 90%).

1. temperatureThe reaction mixture was cooled to room temperature
2. filtrationThe precipitate was collected via filtration
3. washwashed with H2O
4. customdried in vacuo