HRID1666453

反应详情

EQUATION

反应方程式

HRID 1666453 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
-40 °C

PROCEDURE

实验过程

2-(3-Bromo-5-methylphenoxy)-5-(trifluoromethyl)pyridine (2 g, 0.006 mol) and triisopropylborate (1.66 mL, 0.0072 mol) were dissolved in toluene (40 mL) and THF (20 mL) and cooled to −78° C. n-BuLi (5.38 mL, 0.006 mol) was added while maintaining the reaction at −70° C. The reaction was stirred for 1 h at −40° C. Gradually the temperature was increased to −20-0° C. and the reaction was quenched with 2NHCl. The reaction mixture was warmed to RT, concentrated and extracted with EtOAc. The organic extract was dried over Na2SO4 and concentrated under reduced pressure to give the title compound (2.16 g).

WORKUP

后处理

  1. additionwas added
  2. temperaturewhile maintaining
  3. customthe reaction at −70° C
  4. temperatureGradually the temperature was increased to −20-0° C.
  5. customthe reaction was quenched with 2NHCl
  6. temperatureThe reaction mixture was warmed to RT
  7. concentrationconcentrated
  8. extractionextracted with EtOAc
  9. extractionThe organic extract
  10. dry with materialwas dried over Na2SO4
  11. concentrationconcentrated under reduced pressure