Potassium Hydroxide → 1-Benzenesulfonylamino-2-iodo-4-methanesulfonylbenzene

HRID 1814069

反応式

HRID 1814069 の反応式
[C:1]1([S:7]([N:10](S(C2C=CC=CC=2)(=O)=O)[C:11]2[CH:16]=[CH:15][C:14]([S:17]([CH3:20])(=[O:19])=[O:18])=[CH:13][C:12]=2[I:21])(=[O:9])=[O:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[OH-].[K+]>O1CCOCC1>[C:1]1([S:7]([NH:10][C:11]2[CH:16]=[CH:15][C:14]([S:17]([CH3:20])(=[O:18])=[O:19])=[CH:13][C:12]=2[I:21])(=[O:8])=[O:9])[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

参加物

4

反応物 2

HCID 14797Potassium HydroxideHCID 225044101-Bisbenzenesulfonylamino-2-iodo-4-methanesulfonylbenzene

生成物 1

HCID 225043761-Benzenesulfonylamino-2-iodo-4-methanesulfonylbenzene収率 93.5%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

反応条件

温度
100 °C

実験手順

To a suspension of the compound obtained in Example 8 (4) (4.90 g) in 1,4-dioxane (85 ml), a 1N aqueous potassium hydroxide solution (21.2 ml) was added and the mixture was stirred at 100° C. for 1 hour. After completion of the reaction, the reaction solution was concentrated under reduced pressure, poured into a saturated aqueous NaCl solution, extracted with tetrahydrofuran, dried over anhydrous sodium sulfate, filtered and concentrated under reduced pressure. The resulting residue was separated using silica gel column chromatography (chloroform:methanol=10:1) to obtain 3.47 g of the desired product in a colorless amorphous form.

後処理

  1. customAfter completion of the reaction
  2. concentrationthe reaction solution was concentrated under reduced pressure
  3. additionpoured into a saturated aqueous NaCl solution
  4. extractionextracted with tetrahydrofuran
  5. dry with materialdried over anhydrous sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated under reduced pressure
  8. customThe resulting residue was separated

出典と根拠

ORDレコード
ord-9bbd8de35dba4319ada54e8359690a58
出典データセット
uspto-grants-2005_04
特許番号
US06875770B2

関連ノート

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