HRID582292

反应详情

EQUATION

反应方程式

HRID 582292 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

4-[1-(3-Nitro-2-pyridyl)piperazin-4-yl-carbonyl]benzoic acid methyl ester (5 g) was dissolved in a co-solvent of methanol (80 ml) and methylene chloride (60 ml) in a pressurized reactor. With the addition of about 1 g of Raney-nickel (50% slurry in water), the reaction mixture was filled with hydrogen gas and stirred at 50~60 psi for 4 hours. After completion of the reaction, reaction mixture was filtered through celite and filtrate was concentrated under reduced pressure. The concentrated residue was treated with hexane and ether for crystallization, filtered, washed and dried to give 4.05 g (yield: 88%) of the desired compound.

WORKUP

后处理

  1. customAfter completion of the reaction, reaction mixture
  2. filtrationwas filtered through celite and filtrate
  3. concentrationwas concentrated under reduced pressure
  4. additionThe concentrated residue was treated with hexane and ether for crystallization
  5. filtrationfiltered
  6. washwashed
  7. customdried