Реакция #440107

Уравнение реакции

ethanol

1-[(5-chloroindol-2-yl)sulfonyl]-4-[[5-(pyridin-4-yl)pyrimidin-2-yl]thiocarbonyl]piperazine

hydrazine monohydrate

→

title compound

1-[(5-Chloroindol-2-yl)sulfonyl]-4-[(hydrazono)[5-(pyridin-4-yl)pyrimidin-2-yl]methyl]piperazine

Растворители

methylene chloride

Условия реакции

Обработка

1. 1
   Другоеat room temperature
2. 2
   workup.DISTILLATIONAfter the solvent was distilled off
3. 3
   Другоеthe residue was purified by chromatography on a silica gel column (8% methanol—methylene chloride)
4. 4
   workup.ADDITIONMethylene chloride was added
5. 5
   Концентрированиеthe resulting mixture was concentrated
6. 6
   ДругоеYellow crystals thus precipitated
7. 7
   Фильтрацияwere collected by filtration
8. 8
   Другоеdried

Методика

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.

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