HRID352925

反应详情

EQUATION

反应方程式

HRID 352925 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

In a mixed solvent of ethanol (100 ml) and methylene chloride (100 ml) was suspended 1-[(5-chloroindol-2-yl)sulfonyl]-4-[[5-(pyridin-4-yl)pyrimidin-2-yl]thiocarbonyl]piperazine (499 mg) at room temperature, followed by the successive addition of hydrazine monohydrate (146 μg) and mercury (II) chloride (272 mg). The resulting mixture was stirred at room temperature for 4 hours. After the solvent was distilled off, the residue was purified by chromatography on a silica gel column (8% methanol—methylene chloride). Methylene chloride was added and the resulting mixture was concentrated. Yellow crystals thus precipitated were collected by filtration and dried, whereby the title compound (100 mg) was obtained.

WORKUP

后处理

  1. customat room temperature
  2. distillationAfter the solvent was distilled off
  3. customthe residue was purified by chromatography on a silica gel column (8% methanol—methylene chloride)
  4. additionMethylene chloride was added
  5. concentrationthe resulting mixture was concentrated
  6. customYellow crystals thus precipitated
  7. filtrationwere collected by filtration
  8. customdried