反应详情

In methanol (100 ml), 1-tert-butoxycarbonyl-4-[(5-chloro-1-phenylsulfonylindol-2-yl)sulfonyl]piperazine (3.63 g) was dissolved. Under ice cooling, a 0.2N methanol solution of sodium hydroxide (100 ml) was added to the resulting solution, followed by stirring at room temperature for 12 hours. After a saturated aqueous solution of ammonium chloride was added to the reaction mixture under ice cooling, water and dichloromethane were added to separate the organic layer. The organic layer was dried over anhydrous sodium sulfate. The solvent was concentrated under reduced pressure. After the solid so precipitated was collected by filtration, it was dissolved in saturated ethanol hydrochloride, followed by stirring for 30 minutes. The reaction mixture was distilled under reduced pressure to remove the solvent, followed by drying under reduced pressure, whereby the title compound (1.25 g, 54%) was obtained as colorless powder.

1. customto separate the organic layer
2. dry with materialThe organic layer was dried over anhydrous sodium sulfate
3. concentrationThe solvent was concentrated under reduced pressure
4. customAfter the solid so precipitated
5. filtrationwas collected by filtration, it
6. dissolutionwas dissolved in saturated ethanol hydrochloride
7. stirringby stirring for 30 minutes
8. distillationThe reaction mixture was distilled under reduced pressure
9. customto remove the solvent
10. dry with materialby drying under reduced pressure, whereby the title compound (1.25 g, 54%)
11. customwas obtained as colorless powder