Реакция #96199

ord-2558f552afc342e5b01cb50080fe971e

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ТемператураAfter cooling with an ice bath
  2. 2
    Фильтрацияacidification with concentrated hydrochloric acid to pH 1.5, the resulting slurry is filtered
  3. 3
    Другоеto yield a slightly brown precipitate which
  4. 4
    Промывкаis washed with 50 ml of water
  5. 5
    Фильтрацияfiltered

Методика

1.58 g of the above 5-(5-trifluoromethyl-2-furylmethylene)rhodanine, 23 ml of 1 N sodium hydroxide solution and 25 ml of water are stirred under nitrogen at room temperature for 10 hours. After cooling with an ice bath and acidification with concentrated hydrochloric acid to pH 1.5, the resulting slurry is filtered to yield a slightly brown precipitate which is washed with 50 ml of water by stirring at room temperature under nitrogen and filtered to yield 0.8 g of slightly brown crystals (yield 60%) of α-mercapto-β-(5-trifluoromethyl-2-furyl)acrylic acid. M.P. 158° C.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US04347255uspto-grants-1982_08