HRID1261198

反应详情

EQUATION

反应方程式

HRID 1261198 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

To a solution of 4-(2-fluoro-4-nitrophenoxy)-5-methyl-5H-pyrrolo[3,2]-4 pyrimidine (29) (253.6 mg, 0.879 mmol) in AcOH (3 mL) at 90° C. was added iron powder (245 mg, 4.4 mmol). The mixture was stirred vigorously for 10 min and filtered. The filtrate was concentrated under reduced pressure to produce a solid, which was dissolved in DCM. The resultant solution was washed with cold NaHCO3 solution and water, dried over Na2SO4 and concentrated to provide a residue which was purified by column chromatography (eluent MeOH—CH2Cl2 1:20) to afford the title compound 30 as a brown solid (120.6 mg, 53% yield). LRMS (M+1) 240.1 (100%).

WORKUP

后处理

  1. filtrationfiltered
  2. concentrationThe filtrate was concentrated under reduced pressure
  3. customto produce a solid, which
  4. washThe resultant solution was washed with cold NaHCO3 solution and water
  5. dry with materialdried over Na2SO4
  6. concentrationconcentrated
  7. customto provide a residue which
  8. customwas purified by column chromatography (eluent MeOH—CH2Cl2 1:20)