HRID492672

反应详情

EQUATION

反应方程式

HRID 492672 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

3-[4-(2-Fluoro-4-nitrophenoxy)pyridin-2-yl]-1-methyl-1-(1-methylpiperidin-4-yl)urea (243 mg) was dissolved in tetrahydrofuran (6 ml)-methanol (6 ml), and then 10% palladium carbon (128 mg) was added thereto under a nitrogen atmosphere, followed by replacing with hydrogen inside the reaction system and stirring for 3 hrs. After replacing with nitrogen inside the system, the catalyst was filtered and washed with methanol. The filtrate was concentrated under a reduced pressure to give a residue, which was then purified by silica gel column chromatography (Fuji Silysia NH, eluent; ethyl acetate) and concentrated under a reduced pressure to provide the titled compound (175 mg, 78.0%) as pale yellow powder.

WORKUP

后处理

  1. filtrationthe catalyst was filtered
  2. washwashed with methanol
  3. concentrationThe filtrate was concentrated under a reduced pressure
  4. customto give a residue, which
  5. customwas then purified by silica gel column chromatography (Fuji Silysia NH, eluent; ethyl acetate)
  6. concentrationconcentrated under a reduced pressure