反应详情

温度

10 °C

Under nitrogen atmosphere, to a solution of 1-benzenesulfonyl-1H-pyrrole (283.9 g) in methylene chloride (1.0 L) were added p-toluoyl chloride (318 g) and boron trifluodie ether complex (350 g), and the mixture was allowed to stand at room temperature for 7 days. The reaction solution was washed twice with IN hydrochloric acid (750 mL), washed with 1N aqueous sodium hydroxide solution (750 mL) and a saturated brine (100 mL), dried, and filtered. The filtrate was concentrated to about a half volume thereof under atmospheric pressure, and thereto was added hexane (500 mL). The mixture was further concentrated, and methylene chloride was evaporated off. The resultant was cooled to 10° C., and the precipitated crystals were collected by filtration, washed with hexane and toluene, and dried to give (1-benzenesulfonyl-1H-pyrrol-2-yl) (4-methylphenyl) ketone (315 g, 71%).

1. washThe reaction solution was washed twice with IN hydrochloric acid (750 mL)
2. washwashed with 1N aqueous sodium hydroxide solution (750 mL)
3. dry with materiala saturated brine (100 mL), dried
4. filtrationfiltered
5. concentrationThe filtrate was concentrated to about a half volume
6. additionunder atmospheric pressure, and thereto was added hexane (500 mL)
7. customwas evaporated off
8. filtrationthe precipitated crystals were collected by filtration
9. washwashed with hexane and toluene
10. customdried