Sodium Hydroxide → 5-Bromo-3-hydroxy-2,3-dihydrobenzothiophene 1,1-Dioxide

HRID 521184노트

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HRID 521184 반응식
[Br:1][C:2]1[CH:3]=[CH:4][C:5]2[S:9](=[O:11])(=[O:10])[CH:8]=[CH:7][C:6]=2[CH:12]=1.[OH-:13].[Na+]>[Cl-].[NH4+]>[Br:1][C:2]1[CH:3]=[CH:4][C:5]2[S:9](=[O:11])(=[O:10])[CH2:8][CH:7]([OH:13])[C:6]=2[CH:12]=1

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 23261743Benzo[b]thiophene, 5-bromo-, 1,1-dioxide

생성물 1

HCID 867293525-Bromo-3-hydroxy-2,3-dihydrobenzothiophene 1,1-Dioxide

시약·촉매·용매 1

HCID 25517Ammonium Chloride용매

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온도
100 °C

실험 절차

5-Bromo-1-benzothiophene 1,1-dioxide (100 mg, 0.41 mmol) was suspended in 1N aqueous sodium hydroxide (2.0 mL), heated to 100° C. in a microwave, and allowed to stir for 15 minutes. The mixture was then allowed to cool to ambient temperature before the mixture was diluted with saturated aqueous ammonium chloride and extracted with EtOAc. The organic layer was washed with brine, dried over anhydrous MgSO4, filtered, and concentrated in vacuo. The residue was used without further purification. LRMS (ESI) calc'd for C8H7BrO3S [M+Na]+: 285. Found: 285.

후처리

  1. temperatureto cool to ambient temperature before the mixture
  2. extractionextracted with EtOAc
  3. washThe organic layer was washed with brine
  4. dry with materialdried over anhydrous MgSO4
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo
  7. customThe residue was used without further purification

출처 및 근거

ORD 기록
ord-12c678c95fcb434c9c8cebfeb29df323
출처 데이터셋
uspto-grants-2016_05
특허 번호
US09328099B2

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