Methyl iodide → 1,2-Benzisothiazole, 5-bromo-2,3-dihydro-2-methyl-, 1,1-dioxide

HRID 1846026ノート

反応式

HRID 1846026 の反応式
[Br:1][C:2]1[CH:3]=[CH:4][C:5]2[S:9](=[O:11])(=[O:10])[NH:8][CH2:7][C:6]=2[CH:12]=1.[C:13](=O)([O-])[O-].[K+].[K+].IC>CCO>[Br:1][C:2]1[CH:3]=[CH:4][C:5]2[S:9](=[O:10])(=[O:11])[N:8]([CH3:13])[CH2:7][C:6]=2[CH:12]=1

参加物

5

反応物 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 706549535-Bromo-2,3-dihydro-1lambda6,2-benzothiazole-1,1-dione

生成物 1

HCID 684304291,2-Benzisothiazole, 5-bromo-2,3-dihydro-2-methyl-, 1,1-dioxide収率 725.7%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a suspension of 5-bromo-2,3-dihydro-1,2-benzisothiazole 1,1-dioxide (200 mg, 0.92 mmol) and potassium carbonate (128 mg, 0.92 mmol) in EtOH (2 mL) was added iodomethane (0.2 mL, 3.2 mmol) and the reaction was stirred at room temperature for 18 hours followed by heating to 50° C. for 2 hours. The reaction was cooled, concentrated in vacuo and diluted with DCM (20 mL). The solution was washed with water (20 mL), dried over Na2SO4 and concentrated in vacuo to afford the title compound as a white solid (1.75 g, 83%).

後処理

  1. temperatureby heating to 50° C. for 2 hours
  2. temperatureThe reaction was cooled
  3. concentrationconcentrated in vacuo
  4. additiondiluted with DCM (20 mL)
  5. washThe solution was washed with water (20 mL)
  6. dry with materialdried over Na2SO4
  7. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-c1ff30b7a5e5470ebe35bfaa3d5b588c
出典データセット
uspto-grants-2015_02
特許番号
US08952008B2

反応ノート

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