HRID1748507

反应详情

EQUATION

反应方程式

HRID 1748507 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

After 1,4-dioxaspiro[4,5]decane-8-carbonitrile (2.5 g) was dissolved in tetrahydrofuran (8 ml), 1M tetrahydrofuran-solution of lithium bis(trimethylsilyl)amide (15 ml) was added at 0° C. and stirred for 30 minutes. 5-Bromo-2-fluoropyridine (2.64 g) was further added and stirred at room temperature for two hours. Water was added to the reaction solution, extracted with ethyl acetate and concentrated in vacuo. The residue was purified with silica gel chromatography (n-hexane/ethyl acetate) and the resulting solid was washed with n-hexane to give the titled compound (3.32 g).

WORKUP

后处理

  1. stirringstirred at room temperature for two hours
  2. extractionextracted with ethyl acetate
  3. concentrationconcentrated in vacuo
  4. customThe residue was purified with silica gel chromatography (n-hexane/ethyl acetate)
  5. washthe resulting solid was washed with n-hexane