HRID1750905

反应详情

EQUATION

反应方程式

HRID 1750905 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a 500 mL Parr Hydrogenator bottle was added 1,2-di(prop-1-en-2-yl)dibenzo[b,d]furan-2-amine (19.1 g, 72.5 mmol), 10% palladium on carbon (5.7 g, 5.36 mmol), 5% platinum on carbon (5.7 g, 1.46 mmol), ethanol (180 mL), and acetic acid (20 mL). The mixture was hydrogenated on a Parr hydrogenator overnight. The reaction mixture was filtered through Celite and washed with dichloromethane. The filtrate was evaporated to brown oil. The oil was dissolved in dichloromethane, washed with 10% sodium hydroxide, dried over magnesium sulfate, filtered, evaporated to a brown oil. The oil was purified using a 200 g Varian column eluting with 10% ethyl acetate/hexanes. 6.55 g (34% yield) of product was obtained.

WORKUP

后处理

  1. customwas hydrogenated on a Parr hydrogenator overnight
  2. filtrationThe reaction mixture was filtered through Celite
  3. washwashed with dichloromethane
  4. customThe filtrate was evaporated to brown oil
  5. dissolutionThe oil was dissolved in dichloromethane
  6. washwashed with 10% sodium hydroxide
  7. dry with materialdried over magnesium sulfate
  8. filtrationfiltered
  9. customevaporated to a brown oil
  10. customThe oil was purified
  11. washeluting with 10% ethyl acetate/hexanes