HRID1986375

反应详情

EQUATION

反应方程式

HRID 1986375 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

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

  1. temperatureAfter cooling rt
  2. washwashed with water and brine
  3. dry with materialThe organic layer was dried over Na2SO4
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo
  6. customThe residue was purified by reverse phase HPLC