Реакция #307666

ord-0795e3ea283f4c93b15e1240568b2a55

Растворители

Условия реакции

Температура
130°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ТемператураCool to ambient temperature
  2. 2
    ЭкстракцияSeparate layers and extract water layer 3 times with DCM
  3. 3
    ПромывкаWash
  4. 4
    Сушкаdry (magnesium sulfate)
  5. 5
    Фильтрацияfilter
  6. 6
    Концентрированиеconcentrated
  7. 7
    Другоеto give the free base of the title
  8. 8
    Другоеpreparation

Методика

Dissolve 1H-pyrazole-4-carboxaldehyde in N,N-dimethylformamide (1.9 mL). Add potassium carbonate (0.539 g, 3.90 mmol) and cyclopropylbromide (0.346 g, 2.86 mmol). Heat in a pressure tube to 130° C. for 18 hr. Cool to ambient temperature and add DCM and water. Separate layers and extract water layer 3 times with DCM. Wash combined DCM layers with brine, dry (magnesium sulfate), filter, and concentrated to give the free base of the title preparation. GC-MS: m/z=136 [M+].

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US08202873B2uspto-grants-2012_06