HRID63723

反应详情

EQUATION

反应方程式

HRID 63723 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

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.

WORKUP

后处理

  1. extractionThe organic compound was extracted into ethyl acetate (2×100 mL)
  2. washthe combined organic layer was washed with brine solution
  3. dry with materialdried over anhydrous MgSO4
  4. filtrationFiltration and concentration
  5. customgave the crude residue which
  6. customwas purified