HRID446010

反应详情

EQUATION

反应方程式

HRID 446010 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of tert-butyl N-(piperidin-4-yl)carbamate (5.3 g, 26.5 mmol), 1-cyclohexane-1-carboxaldehyde (3.5 g, 31.8 mmol), sodium triacetoxyborohydride (7.29 g, 34.4 mmol), acetic acid (0.5 ml) and tetrahydrofuran (dehydrated) (80 ml) was stirred at room temperature for 85 hours and 30 minutes. Water and sodium bicarbonate were added to the reaction mixture, which was stirred and then extracted with ethyl acetate twice. The organic layer was washed with brine and dried over anhydrous sodium sulfate, and the solvent was distilled off. The residue was purified by silica gel column chromatography (NH silica gel, elution solvent: ethyl acetate/heptane) to give the title compound (7.47 g, yield: 95.7%).

WORKUP

后处理

  1. stirringwas stirred
  2. extractionextracted with ethyl acetate twice
  3. washThe organic layer was washed with brine
  4. dry with materialdried over anhydrous sodium sulfate
  5. distillationthe solvent was distilled off
  6. customThe residue was purified by silica gel column chromatography (NH silica gel, elution solvent: ethyl acetate/heptane)