Реакция #1687622

ord-60edf243ccb0493086a32b0c8e78a6a2

Реагенты

Нет

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Другоеuntil acidic reaction
  2. 2
    ФильтрацияThe precipitate was filtered off
  3. 3
    Другоеdried
  4. 4
    workup.DISSOLUTIONdissolved in methanol (25 ml)
  5. 5
    workup.ADDITION5% palladium on charcoal (0.6 g) was added
  6. 6
    ФильтрацияThe catalyst was filtered off
  7. 7
    Другоеthe filtrate was evaporated to dryness
  8. 8
    ДругоеCrystallization from ethanol

Методика

To a solution of 12 (1.93 g, 0.012 mol) in acetone (50 ml) was added hydrogen chloride in ether until acidic reaction. The precipitate was filtered off, dried, and dissolved in methanol (25 ml). 5% palladium on charcoal (0.6 g) was added, and the mixture was shaked overnight under 3 atm. of hydrogen pressure. The catalyst was filtered off and the filtrate was evaporated to dryness. Crystallization from ethanol yielded 0.63 g (0.0031 mol, 26%) of title product M.P. 168°-172° C. Anal. (C7H14ClN5) C, H, N.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: USRE036374uspto-grants-1999_11