HRID1255737

反应详情

EQUATION

反应方程式

HRID 1255737 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

To a solution of 2,6-dichloro-nicotinamide (1) (4 g, 20.9 mmol) in acetonitrile (anhydrous, 60 mL) were added tert-butylamine (2) (13.28 mL, 12.6 mmol) and triethylamine (15.7 mL, 12.6 mmol). The reaction was heated at 80° C. for 2 days. The solution was cooled to room temperature and the resulting suspension was filtered. The filtrate was concentrated in vacuo. The residue was purified by Biotage silica gel chromatography with 20%-100% EtOAc/hexanes gradient elution to afford 850 mg (18% yield) of the title compound.

WORKUP

后处理

  1. temperatureThe solution was cooled to room temperature
  2. filtrationthe resulting suspension was filtered
  3. concentrationThe filtrate was concentrated in vacuo
  4. customThe residue was purified by Biotage silica gel chromatography with 20%-100% EtOAc/hexanes gradient elution