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

HRID 1432225

반응식

HRID 1432225 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

HCID 225043761-Benzenesulfonylamino-2-iodo-4-methanesulfonylbenzene수율 93.5%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

반응 조건

온도
100 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-c2beb6701acc43f49c5f05ef90ada253
출처 데이터셋
uspto-grants-2009_11
특허 번호
US07612070B2

연결된 노트

불러오는 중…