HRID1612707

反应详情

EQUATION

反应方程式

HRID 1612707 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A mixture of 4.55 g of anhydrous triethylamine and 5.0 g of ethyl ethylphosphinate in 100 ml of anhydrous tetrahydrofuran under an inert atmosphere is treated with 4.89 g of chlorotrimethylsilane. The resulting suspension is stirred for 20 hours at room temperature and the solid removed by filtration. Concentration in vacuo affords a cloudy, colourless oil which is treated with 5.10 g of anhydrous N-(2,3-epoxypropyl)phthalimide and 1.0 g of anhydrous zinc chloride. The mixture is heated to 66° C. under an inert atmosphere for 3 hours, cooled to 20° and diluted with dichloromethane. The organic solution is washed with 100 ml of a 10% aqueous sodium bicarbonate solution and dried over anhydrous magnesium sulphate. Removal of the solvents and chromatography on silica gel affords ethyl 3-phthalimido-2-trimethylsilyloxy-propyl(ethyl)phosphinate as a viscous oil.

WORKUP

后处理

  1. customthe solid removed by filtration
  2. concentrationConcentration in vacuo
  3. customaffords a cloudy, colourless oil which
  4. temperatureThe mixture is heated to 66° C. under an inert atmosphere for 3 hours
  5. temperaturecooled to 20°
  6. washThe organic solution is washed with 100 ml of a 10% aqueous sodium bicarbonate solution
  7. dry with materialdried over anhydrous magnesium sulphate
  8. customRemoval of the solvents and chromatography on silica gel