HRID1429244

反应详情

EQUATION

反应方程式

HRID 1429244 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

PROCEDURE

实验过程

4,4′-(1-(4-tert-Butylphenyl)pyrrolidine-2,5-diyl)bis(N-(4-methoxybenzyl)-2-nitroaniline) (2 g, 2.79 mmol) was dissolved in a mixture of THF (15 mL), ethanol (15 mL), and ethyl acetate (5 mL). Then platinum oxide (0.254 g, 1.12 mmol) was added as a THF slurry. The flask was evacuated and purged with nitrogen twice, then evacuated and opened to a hydrogen balloon. The mixture was stirred at room temperature for 20 hours, then filtered through diatomaceous earth, concentrated, and purified by chromatography on silica gel with an 80 g column, eluting with 0-40% ethyl acetate/dichloromethane to give the first peak of trans product (0.508 g, 28%).

WORKUP

后处理

  1. customThe flask was evacuated
  2. custompurged with nitrogen twice
  3. customevacuated
  4. filtrationfiltered through diatomaceous earth
  5. concentrationconcentrated
  6. custompurified by chromatography on silica gel with an 80 g column
  7. washeluting with 0-40% ethyl acetate/dichloromethane