반응 #319104

반응 방정식

chlorotrimethylsilane

triethylamine

cyclooctanone

n-hexane

→

1-cyclooctenyloxytrimethylsilane

수율 80.0%

용매

dimethylformamide

dimethylformamide

반응 조건

후처리

1. 1
   기타At the end of the reaction
2. 2
   세척washed twice with 300 ml of a saturated aqueous sodium bicarbonate solution
3. 3
   세척The mixture was washed
4. 4
   온도under cooling with 180 ml of 1.5N hydrochloric acid
5. 5
   세척washed sequentially with an aqueous sodium bicarbonate solution, water, and saline
6. 6
   건조dried with magnesium sulfate
7. 7
   농축The mixture was concentrated
8. 8
   workup.DISTILLATIONdistilled under vacuum

실험 절차

To a solution of 42 g (0.38 mol) of chlorotrimethylsilane and 78 g of triethylamine in 100 ml of dimethylformamide, a solution of 32 g (0.254 mol) of cyclooctanone in 40 ml of dimethylformamide was added. The resultant mixture was stirred at 100° to 115° C. for 48 hours. At the end of the reaction, the reaction mixture was combined with 240 ml of n-hexane and washed twice with 300 ml of a saturated aqueous sodium bicarbonate solution. The mixture was washed under cooling with 180 ml of 1.5N hydrochloric acid, then washed sequentially with an aqueous sodium bicarbonate solution, water, and saline and then dried with magnesium sulfate. The mixture was concentrated and distilled under vacuum, to afford 40 g (80% yield) of 1-cyclooctenyloxytrimethylsilane having a boiling point of 82° to 84° C./5 mmHg.

출처