Реакция #3255

ord-b9d97a55e700483bba5a21fd55b4d6fd

Условия реакции

Температура
60°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Другоеobtained in reference example 2
  2. 2
    Экстракцияextracted with chloroform
  3. 3
    СушкаThe chloroform layer was dried over magnesium sulfate
  4. 4
    Другоеevaporated
  5. 5
    ДругоеThe residue was purified by silica gel column chromatography (eluent; chloroform:methanol=10:1(v/v)) and
  6. 6
    Другоеcrystallized from ethyl acetate

Методика

To a solution prepared with sodium (1.78 g, 77.4 mmol) and 2-dimethylaminoethanol (80 ml, 796 mmol) was added 6-chloro-9,10-methylenedioxy-7H-indeno[2,1-c]quinoline-7-on (8 g, 25.8 mmol) obtained in reference example 2, and the mixture was stirred with heat at 60° C. for 24 hours. The reaction mixture was poured into ice water and extracted with chloroform. The chloroform layer was dried over magnesium sulfate and evaporated. The residue was purified by silica gel column chromatography (eluent; chloroform:methanol=10:1(v/v)) and crystallized from ethyl acetate to give 6.37 g (yield: 68.1%) of title compound. The physicochemical properties thereof are shown in table 2.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US05733918uspto-grants-1998_03