반응 #42385

ord-a9579004e9f04cb59d99e1905f5daad8

반응 조건

온도
0°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타the phases are separated
  2. 2
    세척The organic phase is washed with water
  3. 3
    건조dried (sodium sulfate)
  4. 4
    여과filtered
  5. 5
    농축concentrated under reduced pressure

실험 절차

To an ice-cold solution of methyl 5-(hydroxymethyl)thiophene-2-carboxylate (375 mg, 2.17 mmol) in methylene chloride (9.0 mL) is added phosphorus tribromide (100 μL, 1.08 mmol) and the reaction mixture is stirred at 0° C. for 0.5 h. Saturated sodium bicarbonate (10 mL) is carefully added to the reaction mixture and the phases are separated. The organic phase is washed with water, dried (sodium sulfate), filtered, and concentrated under reduced pressure to yield the title compound in pure form. ESI MS m/z 235 [M+H]+.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07727997B2uspto-grants-2010_06