HRID1368591

反应详情

EQUATION

反应方程式

HRID 1368591 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 4-(tert-butyl)-N-(1-methyl-4-(4-methylphenyl)-3-{2-[(5-nitro-2-pyrimidinyl)oxy]ethoxy}-1H-pyrazol-5-yl)benzenesulfonamide (Example 36) (1276 mg) in ethanol (20 ml) was placed under an atmosphere of hydrogen at 50 psi for 12 hrs using palladium on carbon (5%) as catalyst. The catalyst was filtered through Celite (30 g), and washed with ethanol (3×10 ml). Concentration of the filtrate under reduced pressure afforded a yellow residue. The crude material was purified by column chromatography on silica gel (150 g), eluting with ethyl acetate:hexane (1:1), to yield the title compound as a yellow solid (569 mg).

WORKUP

后处理

  1. filtrationThe catalyst was filtered through Celite (30 g)
  2. washwashed with ethanol (3×10 ml)
  3. customConcentration of the filtrate under reduced pressure afforded a yellow residue
  4. customThe crude material was purified by column chromatography on silica gel (150 g)
  5. washeluting with ethyl acetate:hexane (1:1)