HRID2093463

反应详情

EQUATION

反应方程式

HRID 2093463 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
110 °C

PROCEDURE

实验过程

The tert-butyl 4,4′-bipiperidine-1-carboxylate (1.27 g, 4.7 mmol) and 2,5-dichloropyrazine (670 mg, 4.5 mmol) were dissolved in NMP (5 ml) at room temperature, and 1,8-diazabicyclo[5.4.0]-undec-7-ene (1 mL, 6.8 mmol) added drop-wise. The mixture was heated at 110° C. for 1 h, allowed to cool to r.t. and diluted with 50 mL of ethyl acetate. The solution was washed with water (10 mL ×1), brine (10 mL ×1), dried over magnesium sulfate, filtered, and concentrated in vac. The residue was purified by chromatography on silica gel with 10% acetone:hexanes to yield the title compound.

WORKUP

后处理

  1. temperatureto cool to r.t.
  2. washThe solution was washed with water (10 mL ×1), brine (10 mL ×1)
  3. dry with materialdried over magnesium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated in vac
  6. customThe residue was purified by chromatography on silica gel with 10% acetone