HRID564067

反应详情

EQUATION

反应方程式

HRID 564067 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

To 7.70 g (24.1 mmol) (4-bromo-2-fluoro-benzyloxy)-tert-butyl-dimethyl-silane (preparation 16a) in 8 mL 1,4-dioxane is added 937 mg (4.82 mmol) Cu(I)-iodide. The reaction mixture is flushed with argon and 7.23 g (48.2 mmol) sodium iodide and 1.03 mL (9.65 mmol) N,N-dimethylethylen-diamine are added. The mixture is stirred at 120° C. for 7 h in a sealed tube. The reaction mixture is diluted at RT with 5% aqueous NH3-solution and the aqueous phase is extracted with EtOAc. The combined organic phase is washed a few times with water, dried over MgSO4, filtered and the solvent is evaporated.

WORKUP

后处理

  1. additionare added
  2. extractionthe aqueous phase is extracted with EtOAc
  3. washThe combined organic phase is washed a few times with water
  4. dry with materialdried over MgSO4
  5. filtrationfiltered
  6. customthe solvent is evaporated