反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
CONDITIONS
反应条件
- 温度
- 70 °C
PROCEDURE
实验过程
In a 1000 ml four-necked flask having a reflux condenser, KPG stirrer and thermometer, 602 g of dry aniline (pKb 9.4) were heated to 120° C. and 200 g of (chloromethyl)triethoxysilane were added in the course of 180 min with stirring and stirring was effected for a further 60 min. Thereafter, the temperature was reduced to 105° C. and 109 g of ethylenediamine (pKb 4.07) were added to the mixture in the course of 10 min with stirring, phase separation occurring. At constant temperature, stirring was effected for a further 30 min, cooling to 70° C. being effected and the heavier ethylenediamine hydrochloride phase then being separated off. 27 g of anhydrous Lupasol G20 (BASF AG) are then added to the upper phase and distilled as described in Example 4. 200 g of N-phenylaminomethyltriethoxysilane (73.2% yield) having a purity of 94.9% are obtained. The chloride value was 8 ppm.
WORKUP
后处理
- customIn a 1000 ml four-necked flask having
- stirringstirring
- customwas reduced to 105° C.
- stirringwith stirring
- customphase separation
- stirringAt constant temperature, stirring
- waitwas effected for a further 30 min
- customthe heavier ethylenediamine hydrochloride phase then being separated off
- addition27 g of anhydrous Lupasol G20 (BASF AG) are then added to the upper phase
- distillationdistilled