Реакция #54396

ord-9d8bb2789cc347999019fe8bb49d8242

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    workup.ADDITIONThe resulting solution was poured slowly
  2. 2
    ФильтрацияThe solid product was filtered
  3. 3
    Другоеpressed dry
  4. 4
    Фильтрацияfiltered
  5. 5
    Другоеdried

Методика

9.0 g (0.025 mole) of 3-methyl-4-(2-pyridylazo)-1-(p-sulfophenyl)-2-pyrazolin-5-one was added in portions with stirring to 70 ml of SOCl2. To this suspension was added dropwise 3 ml of dimethylformamide. The mixture was stirred overnight. The resulting solution was poured slowly with vigorous stirring into 500 ml of ice water. The solid product was filtered and pressed dry. This product was slurried in 50 percent tetrahydrofuran/ethyl ether, filtered, and dried to obtain 5.3 g (56 percent) of orange solid.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US04148641uspto-grants-1979_04