HRID68459
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
3,4,6-Trichloro-pyridazine (34.39 g, 187.5 mmol) in 100 mL acetic acid was heated at reflux for three hours. The resulting mixture was cooled to room temperature and filtered. The filtrate was diluted with ethylacetate. This was washed three times with water, washed with brine, dried over anhydrous MgSO4, concentrated in vacuo, and purified by flash chromatography (30% ethylacetate/hexanes) to yield 4,6-Dichloro-2H-pyridazin-3-one (6.143 g, 37.23 mmol). MS (ESI) 165.0 (M+H)+.
WORKUP
后处理
- temperatureat reflux for three hours
- filtrationfiltered
- additionThe filtrate was diluted with ethylacetate
- washThis was washed three times with water
- washwashed with brine
- dry with materialdried over anhydrous MgSO4
- concentrationconcentrated in vacuo
- custompurified by flash chromatography (30% ethylacetate/hexanes)