Reaktion #340060

Reaktionsgleichung

tetraethylammonium hydroxide

2-(3,4-epoxycyclohexyl) ethyl trimethoxy silane

tetraethoxy silane

phenyl trimethoxy silane

→

PGMEA

Ausbeute 100.0%

Lösungsmittel

water

ethanol

ethyl acetate

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONTo this mixture was added dropwise
2. 2
   workup.STIRRINGAfter that, the solution was stirred for 2 hours at 40 degrees C
3. 3
   Sonstigethe reaction was quenched
4. 4
   workup.ADDITIONby adding 35 g of acetic acid, and ethanol
5. 5
   Sonstigewas removed under a reduced pressure
6. 6
   SonstigeTo thus-obtained solution
7. 7
   Sonstigea water layer was separated
8. 8
   WaschenAn organic layer was washed twice with ultrapure water
9. 9
   workup.ADDITIONTo this contents was added 600 g of propylene glycol monomethyl ether acetate (PGMEA)
10. 10
    Sonstigeunder a reduced pressure to remove ethyl acetate

Vorschrift

In a 3000 ml glass flask, 1400 g of ethanol, 700 g of pure water, and 50 g of 25% tetraethylammonium hydroxide were placed, and stirred. To this mixture was added dropwise a mixture of 79 g of 2-(3,4-epoxycyclohexyl) ethyl trimethoxy silane, 70 g of tetraethoxy silane, and 14 g of phenyl trimethoxy silane at a liquid temperature of 40 degrees C. After that, the solution was stirred for 2 hours at 40 degrees C. After the reaction finished, the reaction was quenched by adding 35 g of acetic acid, and ethanol was removed under a reduced pressure. To thus-obtained solution was added 2000 ml of ethyl acetate, and a water layer was separated. An organic layer was washed twice with ultrapure water. To this contents was added 600 g of propylene glycol monomethyl ether acetate (PGMEA), and the contents were heated up to a liquid temperature of 40 degrees C. under a reduced pressure to remove ethyl acetate and to give a PGMEA solution of a polymer.

Quelle