HRID470616

反应详情

EQUATION

反应方程式

HRID 470616 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 4-oxo-piperidine-1-carboxylic acid tert-butyl ester (compound of Example 13; 13.5 g, 67 mmol), anhydrous potassium carbonate (11.22 g, 81 mmol) and cyanomethyl phosphonic acid diethylester (15.6 g, 88 mmol) in THF (70 mL) was heated at reflux for 12 h. THF was evaporated and the residue was dissolved in chloroform (2×50 mL). The resulting solution was washed with water (2×50 mL) and brine (50 mL). The organic phase obtained was dried over anhydrous sodium sulphate and concentrated to afford the title compound.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureat reflux for 12 h
  3. customTHF was evaporated
  4. dissolutionthe residue was dissolved in chloroform (2×50 mL)
  5. washThe resulting solution was washed with water (2×50 mL) and brine (50 mL)
  6. customThe organic phase obtained
  7. dry with materialwas dried over anhydrous sodium sulphate
  8. concentrationconcentrated