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

HRID 352806ノート

反応式

HRID 352806 の反応式
[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

参加物

3

反応物 1

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

反応条件

温度
80 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-50f09e0695bb4a8e966c0ec1b61eb907
出典データセット
uspto-grants-2004_06
特許番号
US06747023B1

反応ノート

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