反応 #92001

反応方程式

DMF

3,5-dichlorophenol

imidazole

triisopropylchlorosilane

→

(3,5-dichlorophenoxy)-triisopropylsilane

収率 97.4%

溶媒

water

反応条件

後処理

1. 1
   抽出The organic compound was extracted into ethyl acetate (2×100 mL)
2. 2
   洗浄the combined organic layer was washed with brine solution
3. 3
   乾燥dried over anhydrous MgSO4
4. 4
   ろ過Filtration and concentration
5. 5
   その他gave the crude residue which
6. 6
   その他was purified

実験手順

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.

出典