HRID22740

反应详情

EQUATION

反应方程式

HRID 22740 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

A mixture of 3-methoxy-6-(3-hydroxy-benzofuran-2-sulfonyl)-pyridazine (2.7 mmol, 820 mg), conc. HCl (2 mL), and dioxane (10 mL) was heated at 100° C. for 2 hours. The reaction mixture was cooled and evaporated to dryness. The dried residue was extracted with EtOAc (2×20 mL). The extract was dried, filtered, and the filtrate was evaporated to a residue, which was purified by silica gel chromatography (eluent:EtOAc:n-hexanes::3:1), triturated with water (10 mL), and filtered to obtain the desired product: 6-(3-hydroxy-benzofuran-2-sulfonyl)-2H-pyridazin-3-one (35%, 284 mg); mp 186° C.-189° C.

WORKUP

后处理

  1. temperatureThe reaction mixture was cooled
  2. customevaporated to dryness
  3. extractionThe dried residue was extracted with EtOAc (2×20 mL)
  4. customThe extract was dried
  5. filtrationfiltered
  6. customthe filtrate was evaporated to a residue, which
  7. customwas purified by silica gel chromatography (eluent:EtOAc:n-hexanes::3:1)
  8. customtriturated with water (10 mL)
  9. filtrationfiltered