HRID2255573

反应详情

EQUATION

反应方程式

HRID 2255573 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of the product of the product of Step E (46 mg, 0.12 mmol) in toluene (2 mL) was added 29 mg (0.14 mmol) of trimethylstannyl azide and the reaction mixture was refluxed for 24 hours. The reaction mixture was concentrated in vacuo. The residue was dissolved in THF and treated with 12N HCl (5 drops) for 5 minutes at room temperature. The mixture was concentrated in vacuo and purified on a silica gel flash chromatography column eluted with CHCl3 /MeOH/NH4OH (80:20:2) to afford 19.6 mg (38%) of the title compound.

WORKUP

后处理

  1. temperaturethe reaction mixture was refluxed for 24 hours
  2. concentrationThe reaction mixture was concentrated in vacuo
  3. dissolutionThe residue was dissolved in THF
  4. additiontreated with 12N HCl (5 drops) for 5 minutes at room temperature
  5. concentrationThe mixture was concentrated in vacuo
  6. custompurified on a silica gel flash chromatography column
  7. washeluted with CHCl3 /MeOH/NH4OH (80:20:2)