反应详情

温度

110 °C

A mixture of ammonium phosphinate (9.18 g) and hexamethyldisilazane (25 mL) was heated at 110° C. for 2 hours. The mixture was cooled in ice, dissolved in dry dichloromethane (120 mL), benzyl chloride (20 g; 14 mL) was added and the mixture allowed to warm to room temperature and stirred 18 hours. The solution was filtered, the solvent evaporated, the residue azeotroped with methanol (2×70 mL), dissolved in toluene (150 mL) containing n-butanol (30 mL) and the solution was boiled under reflux in a Dean and Stark water trap for 5 hours. The solvent was evaporated, the residue slurried with dichloromethane (120 mL), filtered and evaporated and the residue chromatographed on silica-gel in 1-2% methanol in dichloromethane to give the title compound as an oil.

1. temperatureThe mixture was cooled in ice
2. temperatureto warm to room temperature
3. filtrationThe solution was filtered
4. customthe solvent evaporated
5. customthe residue azeotroped with methanol (2×70 mL)
6. dissolutiondissolved in toluene (150 mL)
7. additioncontaining n-butanol (30 mL)
8. temperatureunder reflux in a Dean and Stark water trap for 5 hours
9. customThe solvent was evaporated
10. filtrationfiltered
11. customevaporated
12. customthe residue chromatographed on silica-gel in 1-2% methanol in dichloromethane