Dimethyl Sulfoxide → 3(m-diethylaminophenoxy)propyl Trimethoxysilane

Temperatur

88 °C

Using the general procedure described in the preceding Example 1, a reactor was charged with 90.75 g (0.55 mole) m-diethylaminophenol, 112 cc dimethylsulfoxide, 120 cc toluene and 43.28 g of a 50% aqueous sodium hydroxide solution. All of the water present in the reactor was removed by azeotropic distillation. The reaction mixture was allowed to cool to 80° C., at which time 109 g (0.55 mole) of chloropropyl trimethoxysilane were gradually added over a period of 2 hours. The temperature of the reaction mixture increased to 88° C. during the addition. Following completion of the addition, external heating was applied to maintain the temperature of the reaction mixture at 80° C. for 16 hours. The reaction mixture was then allowed to cool and was filtered. The liquid phase was recovered and evaporated under a pressure of 5 mm of mercury to remove the toluene and dimethylsulfoxide. The pressure inside the reactor was reduced to 2 mm and the product, 3(m-diethylaminophenoxy)propyl trimethoxysilane, distilled at a temperature of 185°-187° C. Analysis by vapor phase chromatography demonstrated that the product was 97% pure.

1. customAll of the water present in the reactor was removed by azeotropic distillation
2. additionwere gradually added over a period of 2 hours
3. additioncompletion of the addition
4. temperatureexternal heating
5. temperatureto maintain the temperature of the reaction mixture at 80° C. for 16 hours
6. temperatureto cool
7. filtrationwas filtered
8. customThe liquid phase was recovered
9. customevaporated under a pressure of 5 mm of mercury
10. customto remove the toluene and dimethylsulfoxide
11. distillationthe product, 3(m-diethylaminophenoxy)propyl trimethoxysilane, distilled at a temperature of 185°-187° C

ORD-Eintrag

ord-6dde650ddd7e42268a8fc88a111cd5fd

Quelldatensatz

uspto-grants-1987_02

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US04645844