HRID1193302

反应详情

EQUATION

反应方程式

HRID 1193302 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

Potassium carbonate (3 eq), L-proline (0.4 eq), CuI (0.2 eq) and 4-bromopyridine (1 eq) were added under a protecting gas atmosphere to a solution of tert-butyl piperidin-4-ylmethyl-carbamate (3 g, 15 mmol) in DMSO. The reaction mixture was heated for 20 h at 100° C. After cooling to room temperature, the mixture was diluted with ethyl acetate and sat. sodium chloride solution and filtered over Celite, and the residue was then washed with ethyl acetate. The phases were separated, dried and concentrated under reduced pressure. The crude product was purified by column chromatography. Yield: 30%

WORKUP

后处理

  1. temperatureAfter cooling to room temperature
  2. filtrationfiltered over Celite
  3. washthe residue was then washed with ethyl acetate
  4. customThe phases were separated
  5. customdried
  6. concentrationconcentrated under reduced pressure
  7. customThe crude product was purified by column chromatography