Реакция #1995871

ord-e8ea2ca0dd7c4b898f87d3385721cb98

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Другоеas a result of which the internal temperature
  2. 2
    Другоеrose to 35° C
  3. 3
    Температураat reflux temperature for 1.25 hours
  4. 4
    workup.STIRRINGstirred at 25° C. for 15 hours
  5. 5
    ФильтрацияThe precipitated solid was filtered off with a suction
  6. 6
    Фильтрацияfilter
  7. 7
    Промывкаwashed twice with 25 m
  8. 8
    ДругоеAfter drying at 40-50° C. under reduced pressure

Методика

13.8 g (0.1 mol) of benzaldehyde methylhydrazone and 62.2 g of toluene were admixed with 23.7 g (0.1 mol) of ethyl 2-ethoxymethylene-4,4-difluoro-3-oxo-butyrate, as a result of which the internal temperature rose to 35° C. The reaction mixture was stirred at reflux temperature for 1.25 hours and then stirred at 25° C. for 15 hours. The precipitated solid was filtered off with a suction filter and washed twice with 25 m; each time of toluene. After drying at 40-50° C. under reduced pressure, 23 g of product were obtained.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US08598222B2uspto-grants-2013_12