反应详情

温度

80 °C

To a solution of 1-[(5-chloro-1-phenylsulfonylindol-2-yl)sulfonyl]-3-(2-methylpropyl)piperazine (2.57 g) in a mixture of 1,4-dioxane and distilled water (100-10 ml) was added a 1N aqueous solution (10.4 ml) of sodium hydroxide. The resulting mixture was stirred at 80° C. for 3 days. After saturated ammonium chloride was added to terminate the reaction, distilled water and ethyl acetate were added. The water layer was extracted three times. The organic layers were combined, dried over anhydrous magnesium sulfate and distilled under reduced pressure to remove the solvent. The residue was subjected to chromatography on a silica gel column (methanol:methylene chloride=1:50), whereby the title compound (0.93 g) was obtained as a brown oil.

1. distillationdistilled water (100-10 ml)
2. additionwas added a 1N aqueous solution (10.4 ml) of sodium hydroxide
3. additionAfter saturated ammonium chloride was added
4. customto terminate
5. customthe reaction
6. distillationdistilled water and ethyl acetate
7. additionwere added
8. extractionThe water layer was extracted three times
9. dry with materialdried over anhydrous magnesium sulfate
10. distillationdistilled under reduced pressure
11. customto remove the solvent
12. customwas obtained as a brown oil