반응 #480747

ord-2048159219f94dcd9461dd6f097d6272

반응 조건

온도
35°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    추출was extracted with chloroform
  2. 2
    세척The organic layer was washed with water
  3. 3
    건조a saturated aqueous solution of sodium bicarbonate, dried over anhydrous sodium sulfate
  4. 4
    농축was concentrated
  5. 5
    기타The residue was purified by column chromatography on silica gel (chloroform:methanol=100:1)

실험 절차

To a solution of 2-phenylethanesulfonamide (3.62 g) in methanesulfonic acid (20 ml)-acetic acid (5 ml) was added a solution of trioxane (582 mg) in trifluoroacetic acid (3 ml)and the mixture was stirred for 3 hours at 35° C. To the reaction mixture was added water and was extracted with chloroform. The organic layer was washed with water and a saturated aqueous solution of sodium bicarbonate, dried over anhydrous sodium sulfate and was concentrated. The residue was purified by column chromatography on silica gel (chloroform:methanol=100:1) to give the title compound (1.78 g) having the following physical data.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US06809092B2uspto-grants-2004_10