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

HRID 1852435ノート

反応式

HRID 1852435 の反応式
[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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 25517Ammonium Chloride溶媒

反応条件

温度
100 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-a709b100a83144a59508c20da3a20b0a
出典データセット
uspto-grants-2015_02
特許番号
US08962608B2

反応ノート

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