HRID1715643

反应详情

EQUATION

反应方程式

HRID 1715643 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 2-[5-(2-cyano-4-fluorophenoxy)-indazol-1-yl]-N,N-dimethylacetamide (0.090 g, 0.266 mmol) in EtOH (0.5 mL) was added CoBr2 (27 μL, 0.005 mmol) followed by [2,2′]bipyridinyl (81 μL, 0.015 mmol). NaBH4 (0.030 g, 0.798 mmol) was added to the mixture and it was stirred at room temperature for 18 hours. The mixture was treated with another portion each of CoBr2, [2,2′]bipyridinyl, and NaBH4 and stirred for another 18 hours. The mixture was quenched with MeOH, followed by acetic acid and then concentrated under reduced pressure. The white residue was partitioned between saturated NaHCO3 and ethyl acetate. The organic layer was filtered and concentrated under reduced pressure to afford 10 mg of white solid (11% yield).

WORKUP

后处理

  1. stirringstirred for another 18 hours
  2. customThe mixture was quenched with MeOH
  3. concentrationconcentrated under reduced pressure
  4. customThe white residue was partitioned between saturated NaHCO3 and ethyl acetate
  5. filtrationThe organic layer was filtered
  6. concentrationconcentrated under reduced pressure