HRID500728

反应详情

EQUATION

反应方程式

HRID 500728 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a suspension of 5-bromo-1-(4-bromophenylsulfonyl)-2-methyl-1H-pyrrolo[2,3-b]pyridine (B-7-5) (4 g, 11.4 mmol) in THF (20 mL) was added aq. NaOH (20 mL) at room temperature. The mixture was heated to reflux overnight. LC-MS showed the reaction was complete. Water (100 mL) and EtOAc (50 mL×3) were added into the mixture. The organic layer was separated, dried over anhydrous Na2SO4 and concentrated to give crude mixture which was purified via prep. HPLC to afford 5-bromo-2-methyl-1H-pyrrolo[2,3-b]pyridine (B-7-6) (1.2 g, 50.2%) as a white solid.

WORKUP

后处理

  1. temperatureThe mixture was heated
  2. temperatureto reflux overnight
  3. customThe organic layer was separated
  4. dry with materialdried over anhydrous Na2SO4
  5. concentrationconcentrated
  6. customto give crude mixture which
  7. customwas purified via prep