反应 #328241

ord-7eb2afd095d64758978e9225e02497c7

反应条件

温度
0°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    workup.WAITat room temperature for 4 h
  2. 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+).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US08648066B2uspto-grants-2014_02