反应详情

温度

42.5 °C

Following the same general procedure described in Example 1, a flask was charged with one mol of isopropylmagnesium chloride in 500 ml of tetrahydrofuran under a dry nitrogen atmosphere and stirred. To this was added 1.05 mol (76.8 g) of diethylamine over a period of one hour. During the addition of the diethylamine to the reaction mixture, the pot temperature was maintained at 40-45° C. After the addition was complete, the reaction mixture was refluxed for 30 minutes to complete the evolution of the gas. The reaction mixture was cooled to a pot temperature of 50° C. and one mol (178 g) of isobutyltrimethoxysilane was added over a period of one hour. The reaction mixture was refluxed at a pot temperature of 75° C. for four hours to complete the reaction. The isobutyl(diethylamino)dimethoxysilane was filtered under a nitrogen atmosphere from the magnesium methoxychloride salt. The salt cake was washed with ether (2×200 ml) to obtain the residual isobutyl(diethylamino)dimethoxysilane. The combined filtrate was distilled to a pot temperature of 100° C. to remove the lighter fraction and the residue distilled under reduced pressure to yield 153 g of isobutyl(diethylamino)dimethoxysilaie as a colorless oil (purity>98%); bp 104° C./30 mm. The total yield was 79% of theoretical.

1. additionAfter the addition
2. temperaturethe reaction mixture was refluxed for 30 minutes
3. additionwas added over a period of one hour
4. temperatureThe reaction mixture was refluxed at a pot temperature of 75° C. for four hours
5. customthe reaction
6. filtrationThe isobutyl(diethylamino)dimethoxysilane was filtered under a nitrogen atmosphere from the magnesium methoxychloride salt
7. washThe salt cake was washed with ether (2×200 ml)