反应详情

82 g of dry morpholine (pKb 5.67) were heated to 120° C. in a 500 ml four-necked flask having a reflux condenser, KPG stirrer and thermometer and 80 g of chloromethyltriethoxysilane were added in the course of 180 min with stirring. After the end of the addition, the temperature was reduced to 105° C. and 226.6 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 and the heavier ethylenediamine hydrochloride phase was then separated off. The upper phase was subjected to fractional distillation without a distillation column. 37 g (45% recovery) of morpholine having a purity of 89.7% and 73.5 g (yield 74.2%) of 4-(triethoxysilylmethyl)-tetrahydro-1,4-oxazine were obtained, the purity of which was determined as 97.3%.

1. additionAfter the end of the addition
2. customwas reduced to 105° C.
3. stirringwith stirring
4. customphase separation
5. stirringAt constant temperature, stirring
6. customthe heavier ethylenediamine hydrochloride phase was then separated off
7. distillationThe upper phase was subjected to fractional distillation without a distillation column