HRID1987461

反应详情

EQUATION

反应方程式

HRID 1987461 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 3.41 g (15.0 mmol) of 7-bromo-5-fluoro-2-methyl-1H-indene in 80 ml of ether, 6.00 ml (15.0 mmol) of 2.5 M nBuLi in hexanes was added. The reaction mixture was stirred for 12 h at room temperature; then, this solution was added dropwise to a solution of 3.88 g (15.0 mmol) of (9H-fluoren-9-yl)chlorodimethylsilane in 80 ml of ether over 1 h at room temperature. The resulting mixture was stirred for 12 h, and then 100 ml of water was added. The organic layer was separated, dried over Na2SO4, and evaporated to dryness. The product was isolated by flash chromatography on Silica Gel 60 (40-63 um, d 30 mm, l 400 mm, eluent: hexanes). Yield 3.71 g (55%).

WORKUP

后处理

  1. stirringThe resulting mixture was stirred for 12 h
  2. customThe organic layer was separated
  3. dry with materialdried over Na2SO4
  4. customevaporated to dryness
  5. customThe product was isolated by flash chromatography on Silica Gel 60 (40-63 um, d 30 mm, l 400 mm, eluent: hexanes)