Tetraethylammonium Hydroxide → Propylene glycol methyl ether acetate

Temperatur

40 °C

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.

1. additionTo this mixture was added dropwise
2. stirringAfter that, the solution was stirred for 2 hours at 40 degrees C
3. customthe reaction was quenched
4. additionby adding 35 g of acetic acid, and ethanol
5. customwas removed under a reduced pressure
6. customTo thus-obtained solution
7. customa water layer was separated
8. washAn organic layer was washed twice with ultrapure water
9. additionTo this contents was added 600 g of propylene glycol monomethyl ether acetate (PGMEA)
10. customunder a reduced pressure to remove ethyl acetate

ORD-Eintrag

ord-d42da8e6633e4c97b7d04ca3b7fa2283

Quelldatensatz

uspto-grants-2011_01

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US07868407B2