反应详情

3-Dimethylamino-1-Propyl Tributylstannyl Ether is prepared from 59.6 gm (0.1 mole) bis(tributyltin) oxide and 20.6 gm (0.2 mole) 3-dimethylamino-1-propanol in 200 ml benzene. This is stirred and heated to reflux in a system that contains a Dean-Starke tube. After 30 minutes refluxing water began to collect in the Dean-Starke tube and after refluxing for 22 hours a total of 1.9 ml of water (theory 1.8 ml) had collected. The benzene is stripped off on a rotating evaporator to provide 77.1 gm of straw colored liquid. This is fractionated at reduced pressure, with 53.0 gm water-white liquid (Percent yield - 67.6) being collected at 135°-139° C. at 0.7 mm. Infrared spectral analysis shows this to be the desired ether.

1. temperatureheated
2. temperatureto reflux in a system that
3. customto collect in the Dean-Starke tube
4. temperatureafter refluxing for 22 hours a total of 1.9 ml of water (theory 1.8 ml)
5. customhad collected
6. customThe benzene is stripped off on a rotating evaporator
7. customto provide 77.1 gm of straw colored liquid
8. custombeing collected at 135°-139° C. at 0.7 mm