HRID876568

反应详情

EQUATION

反应方程式

HRID 876568 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of compound 9-4 (70 mg) in AcOH—H2O (2 mL-0.1 mL), was added electrolytic iron powder (95.3 mg). The reaction mixture was stirred at room temperature for 1 hour then at 40° C. for 2 hours to complete the reaction. The reaction mixture was filtered with Celite® pad to remove iron powder. The filtrate was concentrated in vacuo. The resulting residue was purified by amino-silica gel flash column chromatography (eluent: CH2Cl2/MeOH=98/2-95/5) to obtain compound 9-5 (30 mg) as a colorless amorphous solid.

WORKUP

后处理

  1. waitat 40° C. for 2 hours to complete
  2. customthe reaction
  3. filtrationThe reaction mixture was filtered with Celite® pad
  4. customto remove iron powder
  5. concentrationThe filtrate was concentrated in vacuo
  6. customThe resulting residue was purified by amino-silica gel flash column chromatography (eluent: CH2Cl2/MeOH=98/2-95/5)