反応 #1605818

反応方程式

tert-butyldimethylchlorosilane

8-(3-Nitro-4-phenylphenoxy)octan-1-ol

imidazole

→

tert-butyldimethyl{[8-(3-nitro-4-phenylphenoxy)octyl]oxy}silane

収率 86.1%

溶媒

tetrahydrofuran

tetrahydrofuran

反応条件

後処理

1. 1
   その他purified water
2. 2
   workup.ADDITIONwas added
3. 3
   その他the reaction
4. 4
   抽出the mixture was extracted with ethyl acetate
5. 5
   洗浄The organic layer was washed with a saturated aqueous solution of sodium bicarbonate
6. 6
   乾燥a saturated aqueous solution of ammonium chloride, and a saturated aqueous solution of sodium chloride, dried over anhydrous magnesium sulfate
7. 7
   濃縮concentrated under reduced pressure
8. 8
   その他The residue was purified by flash column chromatography

実験手順

8-(3-Nitro-4-phenylphenoxy)octan-1-ol (1.23 g, 3.5 mmol) and imidazole (408 mg, 6.0 mmol) were dissolved in tetrahydrofuran (15 mL) and a solution of tert-butyldimethylchlorosilane (750 mg, 5.0 mmol) in tetrahydrofuran (5 mL) was added thereto. After stirring the reaction mixture at room temperature for 18 hours, purified water was added to stop the reaction and the mixture was extracted with ethyl acetate. The organic layer was washed with a saturated aqueous solution of sodium bicarbonate, a saturated aqueous solution of ammonium chloride, and a saturated aqueous solution of sodium chloride, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The residue was purified by flash column chromatography to obtain tert-butyldimethyl{[8-(3-nitro-4-phenylphenoxy)octyl]oxy}silane (1.38 g).

出典