HRID1986375
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
- 170 °C
PROCEDURE
实验过程
Under Ar, a suspension of the product from Example 9, Step 2 (18.9 mg, 61.1 μmol) in DMF (1 mL) was treated with benzylamine (12 μl, 110 μmol), copper iodide (2.3 mg, 12.2 μmol), phenyl 2-hydroxybenzoate (6.6 mg, 30.6 μmol), and potassium carbonate (16.9 mg, 122.2 μmol). This mixture was then heated to 170° C. by microwave for 40 min. After cooling rt, the reaction mixture was diluted with ethyl acetate and washed with water and brine. The organic layer was dried over Na2SO4, filtered and concentrated in vacuo. The residue was purified by reverse phase HPLC to give the title compound (2.6 mg, 10%). MS (ES+) m/e 336 [M+H]+.
WORKUP
后处理
- temperatureAfter cooling rt
- washwashed with water and brine
- dry with materialThe organic layer was dried over Na2SO4
- filtrationfiltered
- concentrationconcentrated in vacuo
- customThe residue was purified by reverse phase HPLC