1-[(5-Chloro-1-phenylsulfonylindol-2-yl)sulfonyl]-3-(2-methylpropyl)piperazine → (5-Chloroindol-2-yl)sulfonyl-3-(2-methylpropyl)piperazine

HRID 352806노트

반응식

HRID 352806 반응식
[Cl:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][CH:10]=1)[N:7](S(C1C=CC=CC=1)(=O)=O)[C:6]([S:20]([N:23]1[CH2:28][CH2:27][NH:26][CH:25]([CH2:29][CH:30]([CH3:32])[CH3:31])[CH2:24]1)(=[O:22])=[O:21])=[CH:5]2>O1CCOCC1>[Cl:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][CH:10]=1)[NH:7][C:6]([S:20]([N:23]1[CH2:28][CH2:27][NH:26][CH:25]([CH2:29][CH:30]([CH3:32])[CH3:31])[CH2:24]1)(=[O:22])=[O:21])=[CH:5]2

참가 물질

3

반응물 1

HCID 227110221-[(5-Chloro-1-phenylsulfonylindol-2-yl)sulfonyl]-3-(2-methylpropyl)piperazine

생성물 1

HCID 22710654(5-Chloroindol-2-yl)sulfonyl-3-(2-methylpropyl)piperazine

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

반응 조건

온도
80 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-50f09e0695bb4a8e966c0ec1b61eb907
출처 데이터셋
uspto-grants-2004_06
특허 번호
US06747023B1

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