反应详情

Into a 500 ml 3-necked flask equipped with a magnetic stirrer, heating mantle, thermometers, a 12 in. distilling column packed with 1/8 in. glass helices, addition funnel, distilling head and receiver was added 179.3 g (1.0 mole) of 3-aminopropyltrimethoxysilane. The flask was heated to 160° C. and from the (heated) addition funnel 160 g (2.16 moles) of t-butanol was slowly added with the simultaneous distillation of methanol/t-butanol to the receivers. The rate of addition of t-butanol was kept slow in order to maintain as high a flask temperature as possible (150°-170° C). Periodic sampling of the flask and lites for gas chromotograph analysis indicated that after 2.16 moles t-butanol had been added, approximately an 80% conversion of 3-aminopropyltrimethoxysilane to Compound A* had been achieved. Distillation of this material with four cuts (94°-100° C. at 20 mm Hg) produced 100 g of 94% pure aminopropyl-t-butoxydimethoxysilane (combined cuts 2, 3, 4). Cut one, enriched in 3-aminopropyltrimethoxysilane was 30 grams.

1. customInto a 500 ml 3-necked flask equipped with a magnetic stirrer
2. temperatureheating mantle
3. distillationdistilling column
4. additionglass helices, addition funnel
5. distillationdistilling head and receiver
6. temperatureto maintain as high a flask temperature as possible (150°-170° C)
7. aliquotPeriodic sampling of the flask and lites for gas chromotograph analysis
8. additionhad been added
9. distillationDistillation of this material with four cuts (94°-100° C. at 20 mm Hg)