HRID1465468

反应详情

EQUATION

反应方程式

HRID 1465468 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

To a solution of 5-bromopyridine-2-carbonitrile (551.3 mg, 3.012 mmol) in anhydrous dimethylformamide (6.0 ml) were added tert-butyl piperazine-1-carboxylate (670.6 mg, 3.601 mmol) and potassium carbonate (829.0 mg, 5.998 mmol). The mixture was stirred at 120° C. for 63 hrs and cooled to room temperature. Ethyl acetate (30 ml) was added, and the precipitate was collected by filtration. Water (30 ml) was added to the filtrate, and the precipitated solid was collected by filtration and dried under reduced pressure to give tert-butyl 4-(6-cyanopyridin-3-yl)piperazine-1-carboxylate (642.9 mg, yield 74.0%) as a slightly yellow solid.

WORKUP

后处理

  1. temperaturecooled to room temperature
  2. filtrationthe precipitate was collected by filtration
  3. additionWater (30 ml) was added to the filtrate
  4. filtrationthe precipitated solid was collected by filtration
  5. customdried under reduced pressure