HRID22740
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureThe reaction mixture was cooled
- customevaporated to dryness
- extractionThe dried residue was extracted with EtOAc (2×20 mL)
- customThe extract was dried
- filtrationfiltered
- customthe filtrate was evaporated to a residue, which
- customwas purified by silica gel chromatography (eluent:EtOAc:n-hexanes::3:1)
- customtriturated with water (10 mL)
- filtrationfiltered