Реакция #64891

ord-b5cecb5335044841b71ce88453132533

Растворители

Условия реакции

Температура
85°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ФильтрацияThe reaction mixture is filtered after 30 minutes
  2. 2
    Концентрированиеconcentrated in vacuo
  3. 3
    workup.ADDITIONThe residue is then diluted with water
  4. 4
    Экстракцияextracted with CH2Cl2
  5. 5
    СушкаThe extract is dried with Na2SO4
  6. 6
    Фильтрацияfiltered
  7. 7
    Концентрированиеconcentrated in vacuo
  8. 8
    ДругоеThe residue is then purified via flash chromatography (MeOH/CH2Cl2)

Методика

Zinc dust (1.3 g, 20 mmol) is added to a solution of the crude product from step A in 20 mL glacial acetic acid maintained at 85° C. The reaction mixture is filtered after 30 minutes and concentrated in vacuo. The residue is then diluted with water, basified with a 1.0N aqueous NaOH solution, and extracted with CH2Cl2. The extract is dried with Na2SO4, filtered and concentrated in vacuo. The residue is then purified via flash chromatography (MeOH/CH2Cl2) to provide the title compound.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US05416087uspto-grants-1995_05