反应详情

温度

900 °C

A mixture of 2.5 g of 1-iodo-3-(methylsulphanylmethyl)benzene, 1.3 g of sodium tert-butoxide, 0.35 mg of [1,1′-bis(diphenylphosphino)ferrocenyl]palladium chloride, 0.79 g of 1,1′-bis(diphenylphosphino)ferrocene, 4 g of piperazine and 100 cm3 of toluene was heated at 900° C. under a nitrogen stream for 24 hours. The reaction mixture was cooled to room temperature and filtered through sintered glass. The filtrate was washed with 250 cm3 of dichloromethane and then concentrated to dryness under reduced pressure (2.7 kPa). The residue obtained was purified by silica gel column chromatography (particle size 0.04-0.06 mm, diameter 4 cm, height 20 cm) under a pressure of 0.5 bar of nitrogen with a mixture of dichloromethane and methanol (90/10 by volume) and then a mixture of dichloromethane and methanol (85/15 by volume) as eluents, 100-cm3 fractions were collected. Fractions 29 to 36 were combined and concentrated to dryness under reduced pressure (2.7 kPa). The oil obtained was distilled in a bulb oven (B.p.=160° C. approximately under a pressure of 0.1 mm of mercury). 0.67 g of 4-[3-(methylsulphanylmethyl)phenyl]piperazine was obtained in the form of a colorless oil.

1. temperatureThe reaction mixture was cooled to room temperature
2. filtrationfiltered through sintered glass
3. washThe filtrate was washed with 250 cm3 of dichloromethane
4. concentrationconcentrated to dryness under reduced pressure (2.7 kPa)
5. customThe residue obtained
6. customwas purified by silica gel column chromatography (particle size 0.04-0.06 mm, diameter 4 cm, height 20 cm) under a pressure of 0.5 bar of nitrogen with a mixture of dichloromethane and methanol (90/10 by volume)
7. additiona mixture of dichloromethane and methanol (85/15 by volume) as eluents
8. custom100-cm3 fractions were collected
9. concentrationconcentrated to dryness under reduced pressure (2.7 kPa)
10. customThe oil obtained
11. distillationwas distilled in a bulb oven (B.p.=160° C. approximately under a pressure of 0.1 mm of mercury)