HRID965987
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
PROCEDURE
实验过程
A suspension of 4,4,4-trifluoro-1-(3-fluoro-4-(1,3-thiazol-4-yl)phenyl)-1,3-butanedione (503 mg, 1.59 mmol) and 5-hydrazino-2-pyridinesulfonamide hydrochloride (392 mg, 1.74 mmol) in ethanol (22 ml) was stirred at reflux for 28 h. After cooling, the solvent was removed and the residue was added water, extracted with ethyl acetate. The extracts was dried (MgSO4) and concentrated. This was purified on silica gel eluting with ethyl acetate/hexane (1:4/1:3/1:2) to afford 172 mg (23.0%) of the titled compound as a yellow solid.
WORKUP
后处理
- temperatureat reflux for 28 h
- temperatureAfter cooling
- customthe solvent was removed
- additionthe residue was added water
- extractionextracted with ethyl acetate
- dry with materialThe extracts was dried (MgSO4)
- concentrationconcentrated
- customThis was purified on silica gel eluting with ethyl acetate/hexane (1:4/1:3/1:2)