反应 #328241
ord-7eb2afd095d64758978e9225e02497c7
反应方程式
反应条件
温度
0°CELSIUS
详细条件
See reaction.notes.procedure_details.
后处理
- 1workup.WAITat room temperature for 4 h
- 2浓缩Concentration and purification by column chromatography on silica (5-10% methanol in dichloromethane)
实验过程
To a suspension of 2-amino-5-bromonicotinic acid (0.35 g, 1.61 mmol) in tetrahydrofuran (5 mL) was added dimethylamine (0.8 mL of a 2M solution in tetrahydrofuran, 1.60 mmol), diethylphosphoryl cyanide (0.29 g, 1.77 mmol), and triethylamine (0.34 g, 3.38 mmol) at 0° C. The mixture was stirred at 0° C. for 30 min and then at room temperature for 4 h. Concentration and purification by column chromatography on silica (5-10% methanol in dichloromethane) gave the title Compound as a white solid. MS (EI) for C8H10BrN3O: 244 (MH+).