HRID658373
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
To a solution of [4-(5-Amino-[1,3,4]oxadiazol-2-yl)-pyridin-3-yl]-(2-floro-4-iodo-phenyl)-amine (150 mg, 0.38 mmol) in ethanol (10 mL) KOH 9212 mg, 3.78 mmol) was added. The reaction mixture was refluxed for 3 hrs. Then, added acetic acid was added to bring the pH to 5. The volatives were stripped and the residue was dissolved in EtOAc, and washed with 5% Na2CO3, and brine, and then dried over anhydrous MgSO4. After filtration and solvent removal the remaining crude product was subjected to silica gel column chromatography (eluent:Hex:ane EtOAc=1:1) to afford the desired product (45 mg). [5.08 min; 394(M+1)]
WORKUP
后处理
- temperatureThe reaction mixture was refluxed for 3 hrs
- additionwas added
- washwashed with 5% Na2CO3, and brine
- dry with materialdried over anhydrous MgSO4
- filtrationAfter filtration and solvent removal the remaining crude product