HRID1408414

反应详情

EQUATION

反应方程式

HRID 1408414 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
-20 °C

PROCEDURE

实验过程

To a solution of chlorotrimethylsilane (3.55 mL, 27.2 mmol) in acetonitrile (70 mL) was added sodium iodide (3.91 g, 27.2 mmol), and the reaction mixture was stirred at −20° C. for 1 h. Then methyl N-[(5-bromo-2-chlorophenyl)methyl]carbamate (3 g, 7.7 mmol; prepared according to U.S. Pat. No. 6,313,071) was added, and the reaction mixture was stirred at room temperature for 16 h. The reaction mixture was then basified with 1 N aqueous sodium hydroxide solution and extracted with ethyl acetate (3×). The organic layers were combined, washed with water and brine and then dried (Na2SO4). The solvent was evaporated to provide the title product (1.4 g).

WORKUP

后处理

  1. customprepared
  2. addition6,313,071) was added
  3. stirringthe reaction mixture was stirred at room temperature for 16 h
  4. extractionextracted with ethyl acetate (3×)
  5. washwashed with water and brine
  6. dry with materialdried (Na2SO4)
  7. customThe solvent was evaporated