HRID1369480

反应详情

EQUATION

反应方程式

HRID 1369480 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 3-methoxy-6-(indole-2-sulfenyl)-pyridazine) (2.92 mmol, 750 mg), N-chloro-succinimide (2.92 mmol, 390 mg) and methanol (15 mL) was stirred overnight at room temperature. Excess methanol was removed and the residue was extracted with EtOAc (3×10 mL). The EtOAc extract was collected, dried, filtered and evaporated to dryness to obtain a residue, which was purified by silica gel chromatography (eluent: hexanes:EtOAc::19:5) to yield 3-methoxy-6-(3-chloro-indole-2-sulfenyl)-pyridazine (40%, 338 mg).

WORKUP

后处理

  1. customExcess methanol was removed
  2. extractionthe residue was extracted with EtOAc (3×10 mL)
  3. extractionThe EtOAc extract
  4. customwas collected
  5. customdried
  6. filtrationfiltered
  7. customevaporated to dryness
  8. customto obtain a residue, which
  9. customwas purified by silica gel chromatography (eluent: hexanes:EtOAc::19:5)