HRID908622

反应详情

EQUATION

反应方程式

HRID 908622 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Under an argon atmosphere, to a solution of the compound (912 mg) obtained in Step 6 and ammonium formate (750 mg) in ethanol (18 ml) was added 10% palladium carbon (912 mg). After stirring under refluxing conditions for 1 hr, the catalyst was filtered off. The filtrate was concentrated under reduced pressure, and the residue was partitioned by adding ethyl acetate and water. The organic layer was washed with water, dried over anhydrous magnesium sulfate, filtrated, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate:n-hexane=10:1-1:2) to give the title compound (625 mg).

WORKUP

后处理

  1. filtrationthe catalyst was filtered off
  2. concentrationThe filtrate was concentrated under reduced pressure
  3. customthe residue was partitioned
  4. additionby adding ethyl acetate and water
  5. washThe organic layer was washed with water
  6. dry with materialdried over anhydrous magnesium sulfate
  7. filtrationfiltrated
  8. concentrationconcentrated under reduced pressure
  9. customThe residue was purified by silica gel column chromatography (ethyl acetate:n-hexane=10:1-1:2)