Reaktion #1263983

Reaktionsgleichung

dibutyltin oxide

2-ethyl-1-butanol

→

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

Ausbeute 99.0%

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONThe flask containing the mixture, which
2. 2
   Sonstigewas attached to an evaporator (R-144, made by Sibata, Japan)
3. 3
   Sonstigeregulator-equipped oil bath (OBH-24, made by Masuda Corporation, Japan)
4. 4
   SonstigeThe outlet of a purge valve of the evaporator
5. 5
   SonstigeThe purge valve of the evaporator
6. 6
   Sonstigewas closed
7. 7
   Sonstigewas set to approximately 157° C.
8. 8
   Sonstigethe flask was immersed in the oil bath and rotation of the evaporator
9. 9
   SonstigeWith the purge valve of the evaporator
10. 10
    workup.WAITleft open
11. 11
    Temperaturrotational agitation and heating
12. 12
    Sonstigethe purge valve was closed
13. 13
    Sonstigewith the pressure in the system at from 80 to 65 kPa, reaction
14. 14
    workup.WAITwas continued for approximately 5 hours
15. 15
    workup.DISTILLATIONwhile distilling off water-
16. 16
    workup.ADDITIONcontaining 2-ethyl-1-butanol
17. 17
    workup.DISTILLATIONthe distillation
18. 18
    SonstigeThe reaction liquid
19. 19
    Sonstige928 g of reaction liquid
20. 20
    Sonstigewas obtained in the flask
21. 21
    Sonstigeresults

Vorschrift

672 g (2.7 mol) of dibutyltin oxide (made by Sankyo Organic Chemicals Co., Ltd., Japan) and 1700 g (16.7 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 approximately 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 then with the pressure in the system at from 80 to 65 kPa, reaction was continued for approximately 5 hours while distilling off water-containing 2-ethyl-1-butanol. Then, the pressure in the system was further reduced and the distillation was continued, and then once 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. 928 g of reaction liquid was obtained in the flask. According to 119Sn-, 1H-, and 13C-NMR analysis results, the product 1,1,3,3-tetrabutyl-1,3-bis(2-ethylbutyloxy)-distannoxane was obtained at a yield of 99% based on the dibutyltin oxide. The same procedure was repeated twelve times, thus obtaining a total of 11200 g of 1,1,3,3-tetrabutyl-1,3-bis(2-ethylbutyloxy)-distannoxane.

Quelle