HRID8267
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 7-methoxy-4-(2-pyridin-2-yl-5,6-dihydro-4H-pyrrolo[1,2-b]pyrazol-3-yl)-quinoline (53 mg, 0.16 mmol) in N,N-dimethylformamide (3 mL) at room temperature is added sodium ethanthiolate (133 mg, 1.6 mmol). The solution is refluxed for 4 h, cooled, and concentrated in vacuo. The residue is dissolved in methanol and loaded onto an SCX column. The column is washed with water, methanol, and 7 N ammonia in methanol. The appropriate fraction is concentrated in vacuo to yield the title compound, 28 mg (56%), as a yellow solid.
WORKUP
后处理
- temperatureThe solution is refluxed for 4 h
- temperaturecooled
- concentrationconcentrated in vacuo
- dissolutionThe residue is dissolved in methanol
- washThe column is washed with water, methanol, and 7 N ammonia in methanol
- concentrationThe appropriate fraction is concentrated in vacuo