反应详情

2-Dimethylamino-2-Methyl-1-Propyl Tributylstannyl Ether is prepared from 59.6 gm (0.1 mole) bis(tributyltin) oxide and 23.4 gm (0.2 mole) 2-dimethylamino-2-methyl-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 water began to collect in the Dean-Starke tube and after 46 hours only 1.6 ml of water (theory 1.8 ml) had collected. Solvent is stripped off on a rotating evaporator to provide 78.3 gm of straw colored liquid. This is fractionated at reduced pressure to collect the desired product, 52.7 gm of water-white liquid (Percent yield - 65), at 132°-137° C. at 0.5 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 and after 46 hours only 1.6 ml of water (theory 1.8 ml)
4. customhad collected
5. customSolvent is stripped off on a rotating evaporator
6. customto provide 78.3 gm of straw colored liquid
7. customto collect the desired product, 52.7 gm of water-white liquid (Percent yield - 65)
8. customat 132°-137° C.