Реакция #4691

ord-973abaec5c9e43889008b8fe153c5b7e

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ФильтрацияThe mixture was filtered
  2. 2
    Фильтрацияfiltered
  3. 3
    Другоеwas dried
  4. 4
    workup.DISSOLUTIONThe product was dissolved in 350 ml of tetrahydrofuran
  5. 5
    Фильтрацияthe solution was filtered
  6. 6
    Концентрированиеconcentrated to a volume of 75 ml
  7. 7
    ТемператураThe mixture was cooled
  8. 8
    Фильтрацияiced and filtered
  9. 9
    Промывкаthe recovered product was washed with tetrahydrofuran
  10. 10
    Другоеdried

Методика

2.85 ml of a 6.4N hydrogen chloride solution in ethanol were added to a solution of 5.1 g of the product of Example 6 in 5.1 ml of ethanol and then isopropyl ether was added thereto. The mixture was filtered and the recovered product was empasted several times with isopropyl ether, filtered and was dried. The product was dissolved in 350 ml of tetrahydrofuran and the solution was filtered and concentrated to a volume of 75 ml. The mixture was cooled, iced and filtered and the recovered product was washed with tetrahydrofuran and dried to obtain 3.3 g of 3-ethyl-5-(4-methoxyphenyl)-4-phenyl-4H-1,2,4-triazole hydrochloride melting towards 150° C. with decomposition.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US04727084uspto-grants-1988_02