HRID2285

反应详情

EQUATION

反应方程式

HRID 2285 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 4-tert-butyl-N-{5-(4-methylphenyl)-6-[2-(4-nitrophenoxy)ethoxy]pyrimidin-4-yl}benzenesulfonamide (383 mg), 10% palladium-carbon (50 mg) and ethanol-tetrahydrofuran (6 ml-3 ml) is subjected to catalytic hydrogenation at room temperature under hydrogen atmosphere (1 atm) for two hours. The catalyst is removed by filtration, and the filtrate is concentrated. The residue is purified by silica gel column chromatography (solvent; chloroform/ethyl acetate=10:1), and recrystallized from ethyl acetate/diisopropyl ether to give N-{6-[2-(4-aminophenoxy)ethoxy]-5-(4-methylphenyl)pyrimidin-4-yl}-4-tert-butylbenzenesulfonamide (358 mg).

WORKUP

后处理

  1. customis subjected to catalytic hydrogenation at room temperature under hydrogen atmosphere
  2. customfor two hours
  3. customThe catalyst is removed by filtration
  4. concentrationthe filtrate is concentrated
  5. customThe residue is purified by silica gel column chromatography (solvent; chloroform/ethyl acetate=10:1)
  6. customrecrystallized from ethyl acetate/diisopropyl ether