HRID1486428

反应详情

EQUATION

反应方程式

HRID 1486428 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 3-chloropropyltriethoxysilane (2.31 g, 9.6 mmol) and tetrabutylamonium iodide (0.020 g, 0.05 mmol) in butanone (25 mL) was added sodium azide (3.120 g, 48 mmol) and the reaction mixture was heated under reflux for 50 h. Filtration over celite was followed by evaporation of the solvent under vacuum. The residue was dissolved in dichloromethane (150 mL) and then washed with water (2 times 20 mL). The organic phase was dried (NaSO4) and evaporated to give the desired product (1.9 g).

WORKUP

后处理

  1. temperaturethe reaction mixture was heated
  2. temperatureunder reflux for 50 h
  3. filtrationFiltration over celite
  4. customwas followed by evaporation of the solvent under vacuum
  5. dissolutionThe residue was dissolved in dichloromethane (150 mL)
  6. washwashed with water (2 times 20 mL)
  7. dry with materialThe organic phase was dried (NaSO4)
  8. customevaporated