HRID500724

反应详情

EQUATION

反应方程式

HRID 500724 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a suspension of 5-bromo-2,3-dimethyl-1-(phenylsulfonyl)-1H-pyrrolo[2,3-b]pyridine (B-6-3) (0.9 g, 2.5 mmol) in THF (30 mL) and MeOH (30 mL) was added aq. NaOH (20%, 19 mL) at room temperature. The mixture was heated to reflux overnight. TLC (Petroleum ether: EtOAc=5:1) showed the reaction was complete. After the solvent was removed under reduced pressure, water (20 mL) and CH2Cl2 (20 mL) were added into the mixture. The organic layer was separated, dried over anhydrous Na2SO4. The mixture was concentrated to give crude mixture which was purified via prep. HPLC to afford 5-bromo-2,3-dimethyl-1H-pyrrolo[2,3-b]pyridine (B-6-4) (0.4 g, 72.4%) as a white solid.

WORKUP

后处理

  1. temperatureThe mixture was heated
  2. temperatureto reflux overnight
  3. customAfter the solvent was removed under reduced pressure, water (20 mL) and CH2Cl2 (20 mL)
  4. additionwere added into the mixture
  5. customThe organic layer was separated
  6. dry with materialdried over anhydrous Na2SO4
  7. concentrationThe mixture was concentrated
  8. customto give crude mixture which
  9. customwas purified via prep