反应详情

In ethanol (50 ml) was suspended 1-[(5-chloroindol-2-yl)sulfonyl]-4-[[5-(pyridin-4-yl)pyrimidin-2-yl]thiocarbonyl]piperazine (243 mg) at room temperature, followed by the successive addition of hydroxylamine hydrochloride (338 mg), sodium acetate (399 mg) and mercury (II) chloride (132 mg). The resulting mixture was stirred at room temperature for 6 hours. The insoluble matter was filtered off through Celite filtration. The residue was purified by chromatography on a silica gel column (7% methanol—methylene chloride), whereby two fractions were obtained. They were concentrated, respectively, whereby a low-polarity compound (20 mg, colorless powder) and a high-polarity compound (20 mg, colorless powder) were obtained. Low-polarity compound:

1. customat room temperature
2. filtrationThe insoluble matter was filtered off through Celite filtration
3. customThe residue was purified by chromatography on a silica gel column (7% methanol—methylene chloride)
4. customwhereby two fractions were obtained
5. concentrationThey were concentrated
6. customrespectively, whereby a low-polarity compound (20 mg, colorless powder) and a high-polarity compound (20 mg, colorless powder) were obtained