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

HRID 1846026노트

반응식

HRID 1846026 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-c1ff30b7a5e5470ebe35bfaa3d5b588c
출처 데이터셋
uspto-grants-2015_02
특허 번호
US08952008B2

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