반응 #1786630

ord-ec12768166f949659066b9ceabab9339

용매

반응 조건

온도
120°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    추출extracted with ethyl acetate
  2. 2
    세척the organic phase was washed with water
  3. 3
    건조dried over sodium sulfate
  4. 4
    기타The solvent was removed under reduced pressure
  5. 5
    기타the crude product was purified by column chromatography

실험 절차

7.7 g (33 mmol) of 4-chloro-3,3-dimethyl-2,3-dihydro-1,2-benzoisothiazole 1,1-dioxide, 8.25 ml (55 mmol) of bromoacetaldehyde diethyl acetal and 7.0 g of potassium carbonate were taken up in 100 ml of dry DMF and stirred at 120° C. for 5 h. The reaction mixture was poured into ice-water and then extracted with ethyl acetate, and the organic phase was washed with water and dried over sodium sulfate. The solvent was removed under reduced pressure, the crude product was purified by column chromatography. 7.5 g (65%) of the product were obtained as an oil in this way.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US06346622B1uspto-grants-2002_02