反应详情

温度

25 °C

893 g (2.48 mol) of di-n-octyl tin oxide (Sankyo Organic Chemicals Co., Ltd., Japan) and 2403 g (23.6 mol) of 2-ethyl-1-butanol were placed in a 5000 mL volumetric eggplant-shaped flask. The flask was attached to an evaporator to which was connected an oil bath equipped with a temperature controller, a vacuum pump and a vacuum controller. The purge valve outlet of the evaporator was connected to a line containing nitrogen gas flowing at normal pressure. After closing the purge valve of the evaporator to reduce pressure inside the system, the purge valve was opened gradually to allow nitrogen to flow into the system and return to a normal pressure. The oil bath temperature was set to about 165° C., the flask was immersed in the oil bath and rotation of the evaporator was started. After heating for about 40 minutes in the presence of atmospheric pressure nitrogen with the purge valve of the evaporator left open, distillation of 2-ethyl-1-butanol containing water began. After maintaining in this state for 7 hours, the purge valve was closed, pressure inside the system was gradually reduced, and excess 2-ethyl-1-butanol was distilled with the pressure inside the system at 74 to 25 kPa. After the fraction no longer appeared, the flask was taken out of the oil bath. After allowing the flask to cool to the vicinity of room temperature (25° C.), the flask was taken out of the oil bath, the purge valve was opened gradually and the pressure inside the system was returned to atmospheric pressure. 1114 g of reaction liquid were obtained in the flask. Based on the results of 119Sn-, 1H- and 13C-NMR analyses, 1,1,3,3-tetra-n-octyl-1,3-bis(2-ethylbutyloxy)distannoxane was confirmed to have been obtained at a yield of 99% based on di-n-octyl tin oxide. The same procedure was then repeated 12 times to obtain a total of 13380 g of 1,1,3,3-tetra-n-octyl-1,3-bis(2-ethylbutyloxy)distannoxane.

1. customThe flask was attached to an evaporator to which
2. customequipped with a temperature controller
3. customThe purge valve outlet of the evaporator
4. additioncontaining nitrogen gas
5. customthe purge valve of the evaporator
6. customwas set to about 165° C.
7. customthe flask was immersed in the oil bath and rotation of the evaporator
8. temperatureAfter heating for about 40 minutes in the presence of atmospheric pressure nitrogen with the purge valve of the evaporator
9. waitleft open
10. distillationdistillation of 2-ethyl-1-butanol
11. additioncontaining water
12. temperatureAfter maintaining in this state for 7 hours
13. customthe purge valve was closed
14. distillationexcess 2-ethyl-1-butanol was distilled with the pressure inside the system at 74 to 25 kPa
15. custom1114 g of reaction liquid
16. customwere obtained in the flask