反应详情

温度

-78 °C

In a 50 ml three-necked flask equipped with a dropping funnel and a magnetic stirrer, 0.36 g (14.8 mmol) of magnesium and 10 ml of anhydrous diethyl ether were charged at room temperature in a nitrogen gas atmosphere. After several drops of 1,2-dibromoethane were added so as to activate magnesium, 2.0 ml (14.2 mmol) of chloromethyltrimethylsilane were added dropwise carefully to avoid heat build-up. When the reaction solution was stirred for 1 hour while it was heated mildly with a drier, the solution darkened. Then, after the solution was cooled to −78° C., 3.0 g (14.2 mmol) of chlorobis(diethylamino)phosphine synthesized in (a) were added dropwise to the solution, and the resultant mixture was then returned to room temperature and refluxed for 1 hour. The resulting crystals were filtered off, washed with anhydrous diethyl ether, and purified by vacuum-distillation (0.2 kPa, 74.3-79.5° C.) to obtain 2.29 g of bis(diethylamino)(trimethylsilylmethyl)phosphine in the form of a colorless transparent liquid; the yield was 62%.

1. customIn a 50 ml three-necked flask equipped with a dropping funnel and a magnetic stirrer
2. additionwere added dropwise carefully
3. temperatureto avoid heat
4. temperaturewas heated mildly with a drier
5. additionwere added dropwise to the solution
6. customwas then returned to room temperature
7. temperaturerefluxed for 1 hour
8. filtrationThe resulting crystals were filtered off
9. washwashed with anhydrous diethyl ether
10. distillationpurified by vacuum-distillation (0.2 kPa, 74.3-79.5° C.)