HRID22727

反应详情

EQUATION

反应方程式

HRID 22727 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 2-mercaptoindole (6.7 mmol, 1.0 g) in acetone (20 mL) was added 2-chloro-6-methoxy-pyridazine (144 mmol, 1.52 g) and potassium carbonate (70 mmol, 0.98 g) and the reaction mixture was refluxed for 2 hours. Excess acetone was removed and the residue was partitioned between CHCl3 (20 mL) and H2O (20 mL). The CHCl3 layer was collected, dried, filtered and the filtrate was evaporated to a residue, which was purified by silica gel chromatography (eluent:hexanes:EtOAc::4:1) to obtain 3-methoxy-6-(indole-2-sulfenyl)-pyridazine (31%, 534 mg).

WORKUP

后处理

  1. temperaturethe reaction mixture was refluxed for 2 hours
  2. customExcess acetone was removed
  3. customthe residue was partitioned between CHCl3 (20 mL) and H2O (20 mL)
  4. customThe CHCl3 layer was collected
  5. customdried
  6. filtrationfiltered
  7. customthe filtrate was evaporated to a residue, which
  8. customwas purified by silica gel chromatography (eluent:hexanes:EtOAc::4:1)