Reaction #1365707

Reaction equation

3-aminopropyltrimethoxysilane

diethyl maleate

N-(3-trimethoxysilyipropyl) aspartic acid diethyl ester

→

Silane Aspartate

Conditions

Workup

1. 1
   Otherfitted with agitator
2. 2
   workup.ADDITIONthermocouple, nitrogen inlet and addition funnel with condenser
3. 3
   TemperatureThe reactor was maintained at 25° C. for an additional 5 hours at which time the product
4. 4
   workup.ADDITIONwas poured into glass containers
5. 5
   Othersealed under a blanket of nitrogen
6. 6
   workup.WAITAfter one week the unsaturation number was
7. 7
   Otherat 25° C.

Procedure

1482 parts (8.27 equiv.) of 3-aminopropyltrimethoxysilane were added to a 5 liter flask fitted with agitator, thermocouple, nitrogen inlet and addition funnel with condenser. 1423.2 parts (8.27 equiv.) of diethyl maleate were added dropwise through the addition funnel over a period of 2 hours. The temperature of the reactor was maintained at 25° C. during the addition. The reactor was maintained at 25° C. for an additional 5 hours at which time the product was poured into glass containers and sealed under a blanket of nitrogen. After one week the unsaturation number was 0.6 indicating the reaction was ˜99% complete. The product, N-(3-trimethoxysilyipropyl) aspartic acid diethyl ester, had a viscosity of 11 mPa.s at 25° C.

Source