HRID2209975

反应详情

EQUATION

反应方程式

HRID 2209975 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
55 °C

PROCEDURE

实验过程

Into a mixed solvent of tetrahydrofuran (800 ml) and methanol (200 ml) was dissolved 4-[2-[4-(1H-indol-3-yl)-1-piperidinyl]ethyl]-6-nitro-2(1H)-quinolinone (III-19) (6 g, 14.4 mmol) under heating. Paladium on carbon (2.5 g) was added thereto and the mixture was stirred under hydrogen atmosphere at 55 ° C. for 4 hours. The reaction mixture was filtered at the same temperature and the solvent was distilled off from the filtrate. The residue was dried and then recrystallized from a mixture of methanol, THF and water to give the desired product (III-20) (4.3 g) as pale yellow crystals (mp 214°-216 ° C. (methanol/tetrahydrofuran water)). Yield 77.3 %.

WORKUP

后处理

  1. temperatureunder heating
  2. additionPaladium on carbon (2.5 g) was added
  3. filtrationThe reaction mixture was filtered at the same temperature
  4. distillationthe solvent was distilled off from the filtrate
  5. customThe residue was dried
  6. customrecrystallized from a mixture of methanol, THF and water