HRID260636

反应详情

EQUATION

反应方程式

HRID 260636 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 2-phenylethylmagnesium bromide, prepared from 2-phenylethyl bromide (9.25 g, 50 mmol) and magnesium (1.34 g, 55 mmol) in tetrahydrofuran (50 ml), is added chlorochlormethyldimethylsilane (6.43 g, 45 mmol) in tetrahydrofuran (25 ml). The mixture is refluxed for 18 hours, cooled to 0° C. and hydrolyzed with 3N HCl (50 ml). The mixture is then poured in water (50 ml) and diethyl ether (50 ml), the organic layer is washed with water, brine, dried over MgSO4 and the solvents removed in vacuo. Fractional distillation affords the title compound (5.15 g, 48.5% yield).

WORKUP

后处理

  1. temperatureThe mixture is refluxed for 18 hours
  2. washdiethyl ether (50 ml), the organic layer is washed with water, brine
  3. dry with materialdried over MgSO4
  4. customthe solvents removed in vacuo
  5. distillationFractional distillation