HRID2415780

反应详情

EQUATION

反应方程式

HRID 2415780 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

2.25 g (0.01 mol) of nitro benzyl alcohol compound was dissolved in a mixture of 45 mL of methanol and 45 mL of THF. A solid ammonium formate was then added (3.18 g, 0.05 mol, 5 equivalents) followed by the careful addition of 455 mg of 10% palladium on carbon. The reaction mixture was then stirred very slowly at room temperature under reflux condenser. Once it starts, the reaction was rapid and exothermic. After about 1 hour the evolution of hydrogen gas ceased and reaction was checked on TLC (more polar product formation, reaction was dome after this time). The crude reaction was then filtered thru celite, the filtrate diluted with four times of its volume of diethyl ether. The white precipitate that formed was filtered off and dried in vacuo. 1.403 g (72%) of off-white solid was collected.

WORKUP

后处理

  1. temperatureunder reflux condenser
  2. customreaction
  3. custommore polar product formation, reaction
  4. customThe crude reaction
  5. filtrationwas then filtered thru celite
  6. additionthe filtrate diluted with four times of its volume of diethyl ether
  7. customThe white precipitate that formed
  8. filtrationwas filtered off
  9. customdried in vacuo
  10. custom1.403 g (72%) of off-white solid was collected