反応 #1263986

反応方程式

dioctyltin oxide

2-ethyl-1-butanol

→

1,1,3,3-tetraoctyl-1,3-bis(2-ethylbutyloxy)-distannoxane

収率 99.0%

反応条件

後処理

1. 1
   workup.ADDITIONThe flask containing the mixture, which
2. 2
   その他was attached to an evaporator (R-144, made by Sibata, Japan)
3. 3
   その他regulator-equipped oil bath (OBH-24, made by Masuda Corporation, Japan)
4. 4
   その他The outlet of a purge valve of the evaporator
5. 5
   その他The purge valve of the evaporator
6. 6
   その他was closed
7. 7
   その他was set to 157° C.
8. 8
   その他the flask was immersed in the oil bath and rotation of the evaporator
9. 9
   その他With the purge valve of the evaporator
10. 10
    workup.WAITleft open
11. 11
    温度rotational agitation and heating
12. 12
    その他the purge valve was closed
13. 13
    workup.ADDITIONwater-containing 2-ethyl-1-butanol
14. 14
    workup.DISTILLATIONwas distilled off with the pressure in the system at from 84 to 65 kPa
15. 15
    温度This state was maintained for 7 hours
16. 16
    workup.DISTILLATIONexcess 2-ethyl-1-butanol was distilled off
17. 17
    その他The reaction liquid
18. 18
    その他883 g of reaction liquid
19. 19
    その他was obtained in the flask
20. 20
    その他results

実験手順

700 g (1.94 mol) of dioctyltin oxide (made by Sankyo Organic Chemicals Co., Ltd., Japan) and 1600 g (15.7 mol) of 2-ethyl-1-butanol (made by Chisso Corporation, Japan) were put into a 3000 mL flask. The flask containing the mixture, which was a white slurry, was attached to an evaporator (R-144, made by Sibata, Japan) having a temperature regulator-equipped oil bath (OBH-24, made by Masuda Corporation, Japan), a vacuum pump (G-50A, made by Ulvac, Japan) and a vacuum controller (VC-10S, made by Okano Works Ltd., Japan) connected thereto. The outlet of a purge valve of the evaporator was connected to a line for nitrogen gas flowing at normal pressure. The purge valve of the evaporator was closed, and the pressure in the system was reduced, and then the purge valve was gradually opened, so as to pass nitrogen into the system, and thus return the system to normal pressure. The oil bath temperature was set to 157° C., and the flask was immersed in the oil bath and rotation of the evaporator was commenced. With the purge valve of the evaporator left open, rotational agitation and heating were carried out for approximately 40 minutes at normal pressure, and then the purge valve was closed, and the pressure in the system was gradually reduced, and water-containing 2-ethyl-1-butanol was distilled off with the pressure in the system at from 84 to 65 kPa. This state was maintained for 7 hours, and then the pressure in the system was further reduced, and excess 2-ethyl-1-butanol was distilled off. Once the distillate stopped coming off, the flask was lifted out from the oil bath. The reaction liquid was a transparent liquid. After lifting the flask out from the oil bath, the purge valve was gradually opened, so as to return the pressure in the system to normal pressure. 883 g of reaction liquid was obtained in the flask. According to 119Sn-, 1H-, and 13C-NMR analysis results, the product 1,1,3,3-tetraoctyl-1,3-bis(2-ethylbutyloxy)-distannoxane was obtained at a yield of 99% based on the dioctyltin oxide. The same procedure was repeated twelve times, thus obtaining a total of 10600 g of 1,1,3,3-tetraoctyl-1,3-bis(2-ethylbutyloxy)-distannoxane.

出典