HRID42302
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 100 °C
PROCEDURE
实验过程
A mixture consisting of 2-phenylpyrimidine-5-carbonitrile (200 mg, 1.10 mmol), sodium azide (80 mg, 1.2 mmol) and ammonium chloride (66 mg, 1.2 mmol) in DMF (3 mL) was stirred at 100° C. for 24 hours. The reaction mixture was allowed to cool to room temperature. Upon addition of 1N hydrochloric acid (3 mL), a white solid precipitated. The precipitate was isolated by filtration and recrystallized from ethanol to afford the title compound as a white solid (123 mg, 50% yield); melting point 237° C.; 1H-NMR (400 MHz; DMSO-d6) δ 9.51 (s, 2H), 8.51-8.53 (m, 2H), 7.61-7.65 (m, 3H); LC/MS (ESI+) m/z 225; H-PGDS FPBA IC50: 2.5 μM.
WORKUP
后处理
- temperatureto cool to room temperature
- customa white solid precipitated
- customThe precipitate was isolated by filtration
- customrecrystallized from ethanol