HRID2088988

反应详情

EQUATION

反应方程式

HRID 2088988 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
150 °C

PROCEDURE

实验过程

To a solution of 2,6-dichloro-4-iodopyridine (0.1 g, 0.36 mmol) was added excess (1 mL) cyclohexylamine. The reaction mixture was heated at 150° C. in a microwave for 20 minutes. The reaction mixture was cooled to room temperature and diluted with ethyl acetate, at which time a white solid precipitated from the solution. The solid was filtered off and the organics were washed with sodium bicarbonate, water, brine, dried over MgSO4, filtered, and concentrated. The residue was purified on silica gel by flash chromatography (gradient elution: 0% to 50% ethyl acetate/hexane) to afford the title compound as an oil. m/z 337.0 (DCI, M+H)+.

WORKUP

后处理

  1. temperatureThe reaction mixture was cooled to room temperature
  2. customprecipitated from the solution
  3. filtrationThe solid was filtered off
  4. washthe organics were washed with sodium bicarbonate, water, brine
  5. dry with materialdried over MgSO4
  6. filtrationfiltered
  7. concentrationconcentrated
  8. customThe residue was purified on silica gel by flash chromatography (gradient elution: 0% to 50% ethyl acetate/hexane)