HRID733678

反应详情

EQUATION

反应方程式

HRID 733678 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
-78 °C

PROCEDURE

实验过程

To a solution of 4-bromo-1-(tert-butyl-dimethyl-silanyl)-7-chloro-1H-pyrrolo[2,3-c]pyridine (500 mg) in dry tetrahydrofuran (25 ml) at −78° C. under an atmosphere of nitrogen was added tert-butyllithium (1.7M in pentane, 1.88 ml). After addition, the reaction mixture was stirred for 15 minutes at −78° C. then poured onto crushed pellets of carbon dioxide. The mixture was allowed to warm to room temperature and then evaporated. The residue was dissolved in water and the aqueous washed twice with diethyl ether. The aqueous was then acidified with 2M hydrochloric acid and extracted twice with ethyl acetate. The organic layer was dried (MgSO4) and evaporated to give the title compound as a yellow solid (120 mg).

WORKUP

后处理

  1. additionAfter addition
  2. additionthen poured
  3. temperatureto warm to room temperature
  4. customevaporated
  5. dissolutionThe residue was dissolved in water
  6. washthe aqueous washed twice with diethyl ether
  7. extractionextracted twice with ethyl acetate
  8. dry with materialThe organic layer was dried (MgSO4)
  9. customevaporated