반응 #92001

반응 방정식

DMF

3,5-dichlorophenol

imidazole

triisopropylchlorosilane

→

(3,5-dichlorophenoxy)-triisopropylsilane

수율 97.4%

용매

water

반응 조건

후처리

1. 1
   추출The organic compound was extracted into ethyl acetate (2×100 mL)
2. 2
   세척the combined organic layer was washed with brine solution
3. 3
   건조dried over anhydrous MgSO4
4. 4
   여과Filtration and concentration
5. 5
   기타gave the crude residue which
6. 6
   기타was purified

실험 절차

To a mixture of 3,5-dichlorophenol (16.3 g, 100 mmol), imidazole (14.98 g, 220 mmol), and triisopropylchlorosilane (21.21 g, 110 mmol) was added DMF (200 mL) at room temperature. The resulting brown solution was stirred for 15 h and then it was diluted with water (500 mL). The organic compound was extracted into ethyl acetate (2×100 mL) and the combined organic layer was washed with brine solution and dried over anhydrous MgSO4. Filtration and concentration gave the crude residue which was purified using an ISCO (400 g) column chromatography to obtain 31.1 g (97%) of (3,5-dichlorophenoxy)-triisopropylsilane as a colorless oil. EI(+)-HRMS m/e calcd. for C15H24Cl2OSi (M)+ 318.0973, obsd. 318.0971.

출처