HRID993423

反应详情

EQUATION

反应方程式

HRID 993423 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

22.4 g (0.10 mol) of triethylphosphonoacetate was dissolved in 500 M of acetonitrile and 30.4 g (0.2 mol) of 1,8-diazabicyclo[5.4.0]undec-7-ene(1,5-5)(DBU) was slowly added thereto. To this solution was slowly added 15.6 g (0.10 mol) of 1-naphthaldehyde dissolved in 20 ml of tetrahydrofuran and the mixture was stirred for 8 hours. The organic solvent was removed by distillation under reduced pressure. The resulting residue was dissolved in ethyl acetate, washed twice with water, dried over magnesium sulfate, concentrated and then subjected to silica gel column chromatography (eluent: n-hexane/ethyl acetate=95/5, v/v) to obtain 20.3 g (0.090 mol, Yield 90%) of the title compound.

WORKUP

后处理

  1. customThe organic solvent was removed by distillation under reduced pressure
  2. dissolutionThe resulting residue was dissolved in ethyl acetate
  3. washwashed twice with water
  4. dry with materialdried over magnesium sulfate
  5. concentrationconcentrated