HRID639622

反应详情

EQUATION

反应方程式

HRID 639622 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

N2,N4-Dibenzyl-3-nitro-6-trifluoromethyl-pyridine-2,4-diamine (15.9 g, 35.6 mmol) was dissolved in a mixture of THF (100 ml) and MeOH (200 ml). Raney Nickel (3.18 g, 20 wt %) was added and the mixture was stirred at room temperature under 80 psi H2 for 1 hour. The mixture was filtered through celite to remove the catalyst and the filtrate was concentrated in vacuo to give an oil. Trituration in MeOH with a small amount of water gave a precipitate which was collected by filtration, washed with cold MeOH and dried in vacuo to give the title compound (9.02 g) as a white solid.

WORKUP

后处理

  1. filtrationThe mixture was filtered through celite
  2. customto remove the catalyst
  3. concentrationthe filtrate was concentrated in vacuo
  4. customto give an oil
  5. filtrationwas collected by filtration
  6. washwashed with cold MeOH
  7. customdried in vacuo