反应详情

To a glass reactor fitted with a motor-driven stirrer, a thermometer, water-cooled reflux condenser and dropping funnel was charged 0.5 moles of 4-t-butylphenylmagnesium bromide in THF (prepared in the usual manner from 4-t-butylbromobenzene, magnesium chips and tetrahydrofuran). While maintaining an atmosphere of nitrogen in the reactor, 64.0 g of 3-chloro-n-propyldimethylchlorosilane (prepared in Step A above) was added dropwise to the reactor over a period of 25 minutes, keeping the temperature between 35°-40° C. After the addition was complete, the mixture was stirred for 1 hour while allowing the reation temperature to drop to ~30°. To this mixture was added 400 ml of a 5 percent aqueous ammonium chloride solution. The organic layer was separated and dried over magnesium sulfate. After evaporation of solvent, the residue, weighing 113.6 g, was distilled under vacuum. The fraction boiling at 110°-120° C. at 0.5 mm was collected. It weighed 93.2 g and was a colorless, oily liquid of refractive index 1.5088 at 23° C. Analysis showed the compound to contain 67.4 percent carbon, 9.2 percent hydrogen and 13.0 percent chlorine. Theory for the compound is 67.0 percent carbon, 9.4 percent hydrogen and 13.2 percent chlorine. Gas chromatography showed the compound to be ~90 percent pure.

1. customTo a glass reactor fitted with a motor-driven stirrer
2. temperaturereflux condenser
3. additionwas added dropwise to the reactor over a period of 25 minutes
4. custombetween 35°-40° C
5. additionAfter the addition
6. customto drop to ~30°
7. customThe organic layer was separated
8. dry with materialdried over magnesium sulfate
9. customAfter evaporation of solvent
10. distillationwas distilled under vacuum
11. customThe fraction boiling at 110°-120° C. at 0.5 mm was collected
12. customat 23° C